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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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All sourcesNASA NTRSDOE OSTI
NASA NTRS1979

Some TEM observations of Al2O3 scales formed on NiCrAl alloys

The microstructural development of Al2O3 scales on NiCrAl alloys has been examined by transmission electron microscopy. Voids were observed within grains in scales formed on a pure NiCrAl alloy. Both voids and oxide grains grew measurably with oxidation time at 1100 C. The size and amount of porosity decreased towards the oxide-metal growth interface. The voids resulted from an excess number of oxygen vacancies near the oxidemetal interface. Short-circuit diffusion paths were discussed in reference to current growth stress models for oxide scales. Transient oxidation of pure, Y-doped, and Zr-doped NiCrAl was also examined. Oriented alpha-(Al, Cr)2O3 and Ni(Al, Cr)2O4 scales often coexisted in layered structures on all three alloys. Close-packed oxygen planes and directions in the corundum and spinel layers were parallel. The close relationship between oxide layers provided a gradual transition from initial transient scales to steady state Al2O3 growth.

Smialek, J.↗
NASA NTRS1979

Some TEM observations of Al2O3 scales formed on NiCrAl alloys

The microstructural development of Al2O3 scales on NiCrAl alloys has been examined by transmission electron microscopy. Voids have been observed within grains in scales formed on a pure NiCrAl alloy. Both voids and oxide grains grew measurably with oxidation time at 1100 C. The size and amount of porosity decreased towards the oxide-metal growth interface. It was postulated that the voids resulted from an excess number of oxygen vacancies near the oxide-metal interface. Short-circuit diffusion paths were discussed in reference to current growth stress models for oxide scales. Transient oxidations of pure, Y-doped, and Zr-doped NiCrAl was also examined. Oriented alpha-(Al,Cr)2O3 and Ni(Al,Cr)2O4 scales often coexisted in layered structures on all three alloys. Close-packed oxygen planes and directions in the corundum and spinel layers were parallel. The close relationships between oxide layers provided a gradual transition from initial transient scales to steady state Al2O3 growth.

Smialek, J.↗
DOE OSTI2025

Final report on assessment of molten salt corrosion testing of unirradiated and ion irradiated advanced manufactured high entropy alloys

Generation IV reactors and future fusion reactor designs have led to more demanding materials performance requirements due to their increased operating temperatures, corrosive coolants, and increased radiation doses compared to the current light-water reactor fleet. Among the innovative nuclear technologies under development, molten salt reactors stand out for their potential to offer superior fuel utilization, intrinsic safety characteristics, and economic viability. Of the proposed Generation IV designs, the gas fast reactor operates at 450 to 850°C and the molten salt reactor operates at 565 to 850°C, with the molten salt reactor design needing molten salt corrosion resistant materials [1, 2]. These increased temperatures and more extreme corrosion environments necessitate higher material performance, such as creep strength, radiation-tolerant microstructures, corrosion resistance, and high-temperature tensile properties. Hastelloy-N, a nickel-based alloy with additions of molybdenum and chromium, has been successfully employed to contain molten fluoride salt at temperatures up to 705°C. However, Hastelloy-N becomes embrittled upon neutron irradiation, primarily due to the accumulation of helium produced by (n,a) transmutation reactions. Furthermore, the corrosive nature of molten fluoride and chloride salts presents a formidable challenge, as these salts can react with and dissolve alloying elements such as Cr, Mo, and Fe, leading to selective leaching, loss of protective oxide layers, and accelerated degradation. High entropy alloys (HEAs) and refractory high entropy alloys (RHEAs) have emerged as a prominent area of interest, due to their ability to achieve tailored chemical compositions for specific applications. Unlike conventional alloys, HEAs are characterized by having multiple principal elements in equimolar or near equimolar ratios, leading to an unconventional alloying strategy [3]. This alloying strategy is believed to promote unique properties, such as single-phase stabilization of chemically compatible elements, lattice distortion effects due to atomic radius differences, and proposed sluggish diffusion effects. For extreme-environment applications, RHEAs have garnered much research interest because of the possibility of creating relatively ductile materials that can operate in extremely high-temperature environments, beyond the operating temperatures where other Ni-based superalloys begin to lose strength [4-6]. Idaho National Laboratory (INL) initiated a joint international effort with the Czech Republic to explore the feasibility of manufacturing HEAs for high-temperature nuclear applications using advanced manufacturing. This effort was funded at INL by the United States Department of Energy's Office of Nuclear Energy under the Advanced Reactor Technologies and Advanced Materials and Manufacturing Technologies (AMMT) Program. The HEAs were specifically designed for the corrosive and irradiation environments experienced in gas-cooled fast reactors, molten salt reactors, and fusion power. These alloys have been manufactured by multiple processes to determine the impact of manufacturing processes on the performance of the alloys in corrosive and irradiation environments. Preliminary molten salt corrosion testing showed that equimolar MoNbTiV and MoNbTi alloys exhibit exceptional performance, with arc-melted variants demonstrating only minimal degradation after 1000 hours of exposure to molten chloride salt at 700°C. Conversely, Nb2TiVZr2 showed significant molten salt corrosion susceptibility and microstructural instability during high-temperature molten salt exposures, and was, therefore deemed unfit for molten salt reactor applications. The MoNbTiV, MoNbTi, and Nb2TiVZr2 alloys were further evaluated through ion irradiation experiments conducted at the Michigan Ion Beam Laboratory at the University of Michigan. The microstructural stability and the evolution of irradiation-induced defects were characterized to assess the irradiation resistance of each of these alloys.

36 - MATERIALS SCIENCE↗
NASA NTRS1988

Influence of alloying elements on the oxidation behavior of NbAl3

NbAL3 is one candidate material for advanced aeropropulsion systems because of its high melting point, low density, and good oxidation resistance. Although NbAl3 has the lowest oxidation rate among the binary Nb-Al alloys, it does not form exclusive layers of protective Al2O3 scales. Recently Perkin et al., have shown the feasibility of forming alumina scales on Nb-Al alloys at greatly reduced Al contents. However, the objective was to maintain the high Al content, and hence low density, while achieving the capability of growing protective alumina scales. Alloy development followed approaches similar to those used successfully for superalloys and oxidation resistant MCrAlY coatings. Among the three elements examined (Ti, Si, and Cr) as ternary additions to Nb-Al3, Cr was the most effective in favoring the selective oxidation of Al. Nb-41Al-8Cr formed exclusive layers of alumina and had a k sub p value of 0.22 mg squared/cm (sup 4)/hr at 1200 C. The addition of 1 wt percent Y to this alloy was also beneficial, resulting in nearly an order of magnitude decrease in K sub p at 1200 C. Further improvements were achieved by adding about 1 wt percent Si to the quaternary alloy. The k sub p value of 0.012 mg squared/cm (sup 4)/hr for Nb-40Al-8Cr-1Y-1Si at 1200 C was identical to the best NiAl + Zr alloys. These NbAl3 alloys also exhibited excellent cyclic oxidation resistance for 100 hr at 1200 C, being nearly equivalent to NiAl + Zr.

Hebsur, M. G.↗
NASA NTRS1989

Influence of alloying elements on the oxidation behavior of NbAl3

NbAl3 is one candidate material for advanced aeropropulsion systems because of its high melting point, low density, and good oxidation resistance. Although NbAl3 has the lowest oxidation rate among the binary Nb-Al alloys, it does not form exclusive layers of protective Al203 scales. Recently Perkin et al., have shown the feasibility of forming alumina scales on Nb-Al alloys at greatly reduced Al contents. However, the objective was to maintain the high Al content, and hence low density, while achieving the capability of growing protective alumina scales. Alloy development followed approaches similar to those used successfully for superalloys and oxidation resistant MCrAly coatings. Among the three elements examined (Ti, Si, and Cr) as ternary additions to Nb-Al3, Cr was the most effective in favoring the selective oxidation of Al. Nb-41Al-8Cr formed exclusive layers of alumina and had a k sub p value of 0.22 mg squared/cm (sup 4)/hr at 1200 C. The addition of 1 wt percent Y to this alloy was also beneficial, resulting in nearly an order of magnitude decrease in K sub p at 1200 C. Further improvements were achieved by adding about 1 wt percent Si to the quaternary alloy. The k sub p value of 0.012 mg squared/cm (sup 4)/hr for Nb-40Al-8Cr-1Y-1Si at 1200 C was identical to the best NiAl + Zr alloys. These NbAl3 alloys also exhibited excellent cyclic oxidation resistance for 100 hr at 1200 C, being nearly equivalent to NiAl + Zr.

Hebsur, M. G.↗
NASA NTRS1974

Method for making conductors for ferrite memory arrays

The ferrite memory arrays are made from pre-formed metal conductors for the ferrite arrays. The conductors are made by forming a thin sheet of a metallizing paste of metal alloy powder, drying the paste layer, bisque firing the dried sheet at a first temperature, and then punching the conductors from the fired sheet. During the bisque firing, the conductor sheet shrinks to 58 percent of its pre-fired volume and the alloy particles sinter together. The conductors are embedded in ferrite sheet material and finally fired at a second higher temperature during which firing the conductors shrink approximately the same degree as the ferrite material.

Heckler, C. H.↗
NASA NTRS1992

Lightweight Protective Coatings For Titanium Alloys

Lightweight coating developed to protect titanium and titanium aluminide alloys and titanium-matrix composite materials from attack by environment when used at high temperatures. Applied by sol-gel methods, and thickness less than 5 micrometers. Reaction-barrier and self-healing diffusion-barrier layers combine to protect titanium alloy against chemical attack by oxygen and nitrogen at high temperatures with very promising results. Can be extended to protection of other environmentally sensitive materials.

Wiedemann, Karl E.↗
NASA NTRS2009

Lattice-Matched Semiconductor Layers on Single Crystalline Sapphire Substrate

SiGe is an important semiconductor alloy for high-speed field effect transistors (FETs), high-temperature thermoelectric devices, photovoltaic solar cells, and photon detectors. The growth of SiGe layer is difficult because SiGe alloys have different lattice constants from those of the common Si wafers, which leads to a high density of defects, including dislocations, micro-twins, cracks, and delaminations. This innovation utilizes newly developed rhombohedral epitaxy of cubic semiconductors on trigonal substrates in order to solve the lattice mismatch problem of SiGe by using trigonal single crystals like sapphire (Al2O3) as substrate to give a unique growth-orientation to the SiGe layer, which is automatically controlled at the interface upon sapphire (0001). This technology is different from previous silicon on insulator (SOI) or SGOI (SiGe on insulator) technologies that use amorphous SiO2 as the growth plane. A cubic semiconductor crystal is a special case of a rhombohedron with the inter-planar angle, alpha = 90 deg. With a mathematical transformation, all rhombohedrons can be described by trigonal crystal lattice structures. Therefore, all cubic lattice constants and crystal planes (hkl) s can be transformed into those of trigonal crystal parameters. These unique alignments enable a new opportunity of perfect lattice matching conditions, which can eliminate misfit dislocations. Previously, these atomic alignments were thought to be impossible or very difficult. With the invention of a new x-ray diffraction measurement method here, growth of cubic semiconductors on trigonal crystals became possible. This epitaxy and lattice-matching condition can be applied not only to SiGe (111)/sapphire (0001) substrate relations, but also to other crystal structures and other materials, including similar crystal structures which have pointgroup rotational symmetries by 120 because the cubic (111) direction has 120 rotational symmetry. The use of slightly miscut (less than plus or minus 10 deg.) sapphire (0001) substrate can be used to improve epitaxial relationships better by providing attractive atomic steps in the epitaxial process.

Choi, Sang↗
DOE OSTI2025

Chemical Vapor Transformation of Lithium Metal: Mechanism and Enhanced Stability

Constructing a stable solid electrolyte interface (SEI) with high productivity and scalability is essential for the practical application of thin Li metal anodes. Here, in this work, we report a chemical vapor transformation (CVT) strategy in which Li metal is exposed to trimethylaluminum (TMA), inducing a rapid and spontaneous surface reaction that forms a robust, multilayered SEI. In situ quartz crystal microbalance (QCM) and quadrupole mass spectrometry (QMS), combined with ex situ X-ray photoelectron spectroscopy (XPS), UV Raman spectroscopy, and density functional theory (DFT) calculations, reveal that TMA removes the native passivation layer, reacts with Li metal, and drives a coupled bulk-surface transformation involving Li–Al interdiffusion. The resulting SEI exhibits a chemically graded structure consisting of an inner Li–Al alloy and an outer amorphous carbon layer formed via demethylation and ligand-exchange pathways. This modified surface exhibits significantly enhanced stability compared to that of bare Li in electrochemical cycling using liquid and solid-state electrolytes. This work unveils a unique surface-mediated bulk transformation mechanism for lithium metal and establishes CVT as a scalable and fundamentally distinct approach for the interfacial engineering of reactive metals.

Li metal↗
DOE OSTI2025

ULTIMATE Phase I project: Development of Niobium-based alloys for Turbine Applications

Current Ni-based alloys used in turbine blade applications are operating at 1100°C which is approximately 90% of the solidus of Ni-based alloys. Further increases in temperature can be achieved only through the use of alloys with higher solidus temperatures such as refractory alloys which include Mo, Nb, W, Ta alloys. Niobium has a unique combination of physical properties that include a high melting point (2468°C), lowest density (8.57 g/cc), and the lowest modulus amongst refractory alloys, a good thermal conductivity that increases from 45 W/mK at room temperature to 62 W/mK at 1093°C, good ductility with fabricability using traditional techniques, high strength, good creep resistance, and general chemical inactivity. Hence niobium alloys offer many advantages for use at the desired temperature of 1300°C. One of the major deterrents to the use of niobium and its alloys at high temperatures is achieving good oxidation resistance. In addition, achieving balanced properties of room temperature strength, ductility, fracture toughness, high temperature strength, and creep resistance required for 1300°C operation at a density of 9 g/cm 3 is extremely challenging since the addition of W which is a potent strengthener increases the density of the alloy. This project seeks to enable the development of a tri-layered turbine blade that can operate continuously at 1300°C with the core of the turbine blade providing good creep resistance, the second layer providing improved oxidation resistance over the core layer, and the third layer being an environmental barrier providing oxidation resistance. The objective of this Phase 1 project was to use computational modeling and advanced characterization tools to develop two classes of Nb alloys which could be used as the core layer and the transition layer. The first class of alloys developed in this project was a Nb-alloy designed to serve as the turbine blade core with excellent room temperature strength, ductility, and high temperature strength and creep resistance required for 1300°C operation. These alloys were designed to contain sufficient solute solution strengthening elements (W, Mo) but constrained by the density of alloy, along with the addition of elements such as Zr, Hf, Ta, C, and N to achieve a combination of primary and secondary carbide precipitation. A total of 38 “creep-resistant” alloys were designed and cast during the duration of the project. Processing techniques were developed to keep the oxygen contents as low as possible with typical oxygen contents less than 250 ppm. One alloy with a density of < 9.5 g/cc was successful in meeting the Phase 2 intermediate project mechanical property milestone requirements of room temperature ductility greater than 1.0%, 1200°C creep strain of less than 3% at 150 MPa and 100 hours in vacuum, and with solidus temperature greater than 1500ᵒC. The second class of alloys was designed to be a Nb-rich alloy with improved oxidation resistance when compared to the core layer and was designed specifically to be compatible with the core layer and the outer environmental barrier coating. This Nb- alloy will be specifically designed to be microstructurally stable at these temperatures when in contact with the core alloy and provide protection against catastrophic failure of the barrier coating. Two alloys were cast and processed but further development was discontinued to focus on the development of the creep resistant alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Influence of artificial aging on corrosion of abraded Al-Zn-Mg-Cu alloys

Surface abrasion has been shown to create altered surface layers (ASLs) that are hundreds of nm thick on all types of Al alloys. Such ASLs have lower corrosion resistance than the underlying substrate of Al-Zn-Mg-Cu alloys. Here, we demonstrate how heat treatments affect the ASL microstructure on abraded Al-Zn-Mg-Cu alloys using transmission electron microscopy and atom probe tomography, and also how the corrosion properties change using electrochemical polarization. Additionally, high temperature treatments on the abraded bulk samples enhance η phase precipitation in the ASL, leading to a decreased Zn content in the ASL solid solution, which ennobles the ASL breakdown potential.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Structural Evolution of Layered Hybrid Lead Iodide Perovskites in Colloidal Dispersions

Controlling the structure of layered hybrid metal halide perovskites, such as the Ruddlesden-Popper (R-P) phases, is challenging because of their tendency to form mixtures of varying composition. Colloidal growth techniques, such as antisolvent precipitation, forms colloidal dispersions with properties that match bulk layered R-P phases, but controlling the composition of these particles remains challenging. Here, we explore the microstructure of particles of R-P phases of methylammonium lead iodide prepared by antisolvent precipitation from ternary mixtures of alkylammonium cations, where one cation can form perovskite phases (CH 3 NH 3 + ) and the other two promote layered structures as spacers (e.g. C 4 H 9 NH 3 + and C 12 H 25 NH 3 + ). We determine that alkylammonium spacers pack with constant methylene density in the R-P interlayer, and exclude interlayer solvent in dispersed colloids, regardless of length or branching. Using this result, we illustrate how the competition between cations that act as spacers between layers, or as grain- terminating ligands, determines the colloidal microstructure of layered R-P crystallites in solution. Optical measurements reveal that quantum well dimensions can be tuned by engineering the ternary cation composition. Transmission synchrotron wide-angle X-ray scattering and small angle neutron scattering reveal changes in the structure of colloids in solvent and after deposition into thin films. In particular, we find that spacers can alloy between R-P layers if they share common steric arrangements, but tend to segregate into polydisperse R-P phases if they do not mix. In conclusion, this study provides a framework to compare the microstructure of colloidal layered perovskites and suggests clear avenues to control phase and colloidal morphology.

14 SOLAR ENERGY↗
DOE OSTI2022

A Phase-Field Study on Internal to External Oxidation Transition in High-Temperature Structural Alloys

Structural alloys applied at high temperatures rely on an external dense layer of oxide scale for protection. As some reactive alloy components are selectively oxidized internally, understanding how these dispersed metal oxide particles reach the surface to form a protective scale—the so-called internal to external oxidation transition—is crucial for designing these alloys. While the literature is replete with experimental studies on oxidation of alloys, there is a lack of computational studies in this realm due to the complex nature of coupled reaction and diffusion processes in multicomponent multi-phase alloy systems. In this work, we apply a recently developed phase-field model to simulate the oxidation processes under different compositions and nucleation scenarios to gain insights into how a continuous oxide scale can be established. The results show that while alloy composition is critical for internal to external oxidation transition, the oxide nuclei size, shape and distribution also have significant impact on the transition kinetics.

36 MATERIALS SCIENCE↗
NASA NTRS2018

Development and Flammability Testing of Magnesium Alloys for Space Applications

This project will be comparing the flammability of select lightweight Mg alloys for use in a simulated ISS environment. It will also be determining the factors that influence flammability of selected alloys in elevated oxygen, including the formation of an oxide layer. The significance of this work is that such alloys can reduce weight saving by up to 30%. This work is adding to knowledge base of lightweight Mg alloys for possible future applications, as no previous flammability testing of Mg alloys have been conducted at elevated oxygen concentrations.

International Space Station↗
NASA NTRS2002

Techniques Optimized for Reducing Instabilities in Advanced Nickel-Base Superalloys for Turbine Blades

The High-Speed Research (HSR) Airfoil Alloy program developed fourth-generation single-crystal superalloys with up to an 85 F increase in creep rupture capability over current production airfoil alloys. Recent results have been generated at the NASA Glenn Research Center on these fourth-generation alloys, but in coated form, for subsonic turbine blade applications under NASA's Ultra-Efficient Engine Technology (UEET) Program. One goal for UEET is to optimize the airfoil alloy/thermal barrier coating system for 3100 F turbine inlet temperatures. The state-of-the art turbine blade airfoil system consists of a superalloy single crystal that provides the basic mechanical performance of the airfoil. A thermal barrier coating is used to reduce the temperature of the base superalloy, and a bondcoat is deposited between the base material and the thermal barrier coating. The bondcoat improves the oxidation and corrosion resistance of the base superalloy and improves the spallation resistance of the thermal barrier coating. A commercial platinum aluminide bondcoat was applied to the HSR-developed alloys, and a diffusion zone developed as a result of interaction between the bondcoat and the superalloy. Optimized strength is obtained for superalloys when the refractory element content is high and the limits of microstructural stability are approached or exceeded slightly. For fourthgeneration alloys, instability leads to the formation of topologically close packed (TCP) phases, which form internally in the superalloy, and a secondary reaction zone (SRZ), which forms under the diffusion zone. There was a concern that excessive quantities of either TCP or SRZ might decrease the mechanical properties of the superalloy, with SRZ thought to be particularly detrimental and its formation unpredictable. Thus, an SRZreduction effort was initiated in the NASA UEET Program so that methods developed during the HSR project could be optimized further to reduce or eliminate the SRZ. An SRZ is a three-phase constituent composed of TCP and stringers of gamma phase in a matrix of gamma prime. An incoherent grain boundary separates the SRZ from the gammagamma prime microstructure of the superalloy. The SRZ is believed to form as a result of local chemistry changes in the superalloy due to the application of the diffusion aluminide bondcoat. Locally high surface stresses also appear to promote the formation of the SRZ. Thus, techniques that change the local alloy chemistry or reduce surface stresses have been examined for their effectiveness in reducing SRZ. These SRZ-reduction steps are performed on the test specimen or the turbine blade before the bondcoat is applied. Stressrelief heat treatments developed at NASA Glenn have been demonstrated to reduce significantly the amount of SRZ that develops during subsequent high-temperature exposures. Stress-relief heat treatments reduce surface stresses by recrystallizing a thin surface layer of the superalloy. However, in alloys with very high propensities to form SRZ, stress relief heat treatments alone do not eliminate SRZ entirely. Thus, techniques that modify the local chemistry under the bondcoat have been emphasized and optimized successfully at Glenn. One such technique is carburization, which changes the local chemistry by forming submicron carbides near the surface of the superalloy. Detailed characterizations have demonstrated that the depth and uniform distribution of these carbides are enhanced when a stress relief treatment and an appropriate surface preparation are employed in advance of the carburization treatment. Even in alloys that have the propensity to develop a continuous SRZ layer beneath the diffusion zone, the SRZ has been completely eliminated or reduced to low, manageable levels when this combination of techniques is utilized. Now that the techniques to mitigate SRZ have been established at Glenn, TCP phase formation is being emphasized in ongoing work under the UEET Program. The limitsf stability of the fourth-generation alloys with respect to TCP phase formation are currently being defined along with high-temperature creep rupture properties. In addition, a regression model is being developed at Glenn for the prediction of the presence of TCP phase in the microstructure and SRZ under the diffusion zone. The model is based on a design-of-experiments methodology with emphasis on the potential synergistic effects of alloying elements.

MacKay, Rebecca A.↗
DOE OSTI2020

Oxygen Adsorption, Subsurface Oxygen Layer Formation and Reaction with Hydrogen on Surfaces of a Pt–Rh Alloy Nanocrystal

The oxygen adsorption and its catalytic reaction with hydrogen on Pt–Rh single crystals were studied at the nanoscale by Field Emission Microscopy (FEM) and Field Ion Microscopy (FIM) techniques at 700 K. Both FEM and FIM use samples prepared as sharp tips, apexes of which mimic a single nanoparticle of catalyst considering their similar size and morphology. Oxygen adsorption on Pt-17.4 at.%Rh samples leads to the formation of subsurface oxygen, which is manifested in the field emission (FE) patterns: for O2 exposure of ~3 Langmuir (L), {113} planes appear bright in the emission pattern, while for higher oxygen doses, i.e. 84 L, the bright regions correspond to the high index planes between the {012} and {011} planes. Formation of subsurface oxygen is probably accompanied by a surface reconstruction of the nanocrystal. The subsurface oxygen can be effectively reacted off by subsequent exposure of the sample to hydrogen gas at 700 K. The hydrogenation reaction was observed as a sudden, eruptive change of the brightness seen on the FE pattern. This reaction resulted in the recovery of the initial field emission pattern characteristic of a clean tip, with {012} facets being the most visible. It was shown that the oxygen accumulation-reduction process is completely reversible. The obtained results indicate that the presence of subsurface species must be considered in the description of reactive processes on Pt–Rh catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗