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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 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Microstructural, Oxidation, and Mechanical Behavior of NbTi-Based Refractory Alloys with 5 to 10 Pct Co, Cr, and Ni Additions

NbTi-based refractory alloys with additions of Co, Cr, and Ni represent an interesting medium-entropy alloy system with potential for protective oxide film formation, high strength, and ductility. This study investigates the microstructural evolution, oxidation behavior, and mechanical properties of NbTi-based alloys containing 5 to 10 at. pct Co, Cr, and Ni. CALPHAD predictions suggest that this composition range can be heat treated to obtain a predominantly body-centered cubic matrix phase. Mechanical properties, including microhardness, yield strength, maximum strength, and specific strength are evaluated through isothermal compression tests conducted between room temperature and 800 °C. The oxidation kinetics of these alloys are assessed through discontinuous oxidation tests. Parabolic oxidation kinetics were observed for NbTi–10Ni and NbTi–5Co, while linear oxidation kinetics were found for NbTi–10Cr and NbTi–10(CoCrNi). Microstructures and oxide layers are characterized using X-ray diffraction, electron backscatter diffraction, energy-dispersive X-ray spectroscopy, and scanning electron microscopy. All alloys exhibit significant mechanical softening between room temperature and 800 °C, with elastic-perfectly plastic flow observed at 800 °C. The addition of 10 pct Cr to NbTi resulted in two BCC phases up to 1050 °C, conflicting with CALPHAD predictions of a single-phase solid solution at this temperature, and resulting in higher flow stress at 800 °C. NbTi–10(CoCrNi) exhibited the lowest flow stress at 800 °C despite having more ‘cocktail effect’ potential and insufficient molar fractions of Co, Cr, or Ni to form a desirable protective oxide film.

36 MATERIALS SCIENCE↗
NASA NTRS1990

On diamond, graphitic and amorphous carbons in primitive extraterrestrial solar system materials

Carbon is among the most abundant elements in the universe and carbon chemistry in meteorites and comets is an important key to understanding many Solar System and interstellar processes. Yet, the mineralogical properties and interrelations between various structural forms of elemental carbon remain ambiguous. Crystalline elemental carbons include rhombohedral graphite, hexagonal graphite, cubic diamond, hexagonal diamond (i.e., lonsdaleite or carbon-2H) and chaoite. Elemental carbon also occurs as amorphous carbon and poorly graphitized (or turbostratic) carbon but of all the forms of elemental carbon only graphite is stable under physical conditions that prevail in small Solar System bodies and in the interstellar medium. The recent discovery of cubic diamond in carbonaceous chondrites and hexagonal diamond in chondritic interplanetary dust particles (IDPs) have created a renewed interest in the crystalline elemental carbons that were not formed by shock processes on a parent body. Another technique, Raman spectroscopy, confirms a widespread occurrence of disordered graphite in the Allende carbonaceous chondrite and in chondritic IDPs. Elemental carbons have also been identified by their characteristic K-edge features in electron energy loss spectra (EELS). However, the spectroscopic data do not necessarily coincide with those obtained by selected area electron diffraction (SAED). In order to interpret these data in terms of rational crystalline structures, it may be useful to consider the principles underlying electron diffraction and spectroscopic analyses. Electron diffraction depends on electron scattering, on the type of atom and the distance between atoms in a crystal lattice. Spectroscopic data are a function of the type of atom and the energy of bonds between atoms. Also, SAED is a bulk sampling technique when compared to techniques such as Raman spectroscopy or EELS. Thus, it appears that combined analyses provide contradictory results and that amorphous, or short-range ordered, carbon identified by conventional TEM imaging and SAED may show evidence for sp(3) bonds in EELS spectra. It is suggested that complex, nanometer-scale, mineralogical interrelations are common to all elemental carbons irrespective of their origin. The subsequent thermal history, or energy balance, will determine the ultimate microstructure.

Rietmeijer, Frans J. M.↗
DOE OSTI2025

The Role of Surface Hydroxyls in Dehydration and Dehydrogenation of Formic Acid on Fe 3 O 4 (001)

Understanding the role of surface structure and hydroxylation in catalytic reactions on metal oxide surfaces is important for developing a mechanistic insight into the complex interface processes. Here, we investigate the reactivity of formic acid on reconstructed Fe 3 O 4 (001) using a combination of X-ray photoelectron spectroscopy, infrared reflection absorption spectroscopy, temperature-programmed reaction spectroscopy, low energy electron diffraction, and electronic structure calculations. We find that formic acid initially dissociates at low temperatures (< 80 K) into bidentate formate and a hydroxyl up to an initial dosed coverage of two HCOOH per Fe 3 O 4 (001) unit cell. At higher temperatures (> 450 K), formate largely decomposes along the dehydration pathway, producing CO and H 2 O, with dehydrogenation to CO 2 being a minority side reaction. As a first step, water formation leads to surface oxygen extraction via the Mars-van Krevelen mechanism. Computational studies reveal formate embedded in oxygen vacancies as a key intermediate in the CO formation mechanism. CO formation proceeds via two reaction pathways with desorption that peaks at 530 K on the hydroxyl-rich surface and 560 K on the hydroxyl-deficient surface. Atomic hydrogen coadsorption experiments and ab initio calculations reveal that the presence of surface hydroxyls reduces the CO formation barrier. Furthermore, these results highlight the complex interactions between substrate and intermediate species occurring during reactions on metal oxide surfaces.

Adsorption↗
NASA NTRS1972

Adhesion, friction, wear, and lubrication research by modern surface science techniques.

The field of surface science has undergone intense revitalization with the introduction of low-energy electron diffraction, Auger electron spectroscopy, ellipsometry, and other surface analytical techniques which have been sophisticated within the last decade. These developments have permitted submono- and monolayer structure analysis as well as chemical identification and quantitative analysis. The application of a number of these techniques to the solution of problems in the fields of friction, lubrication, and wear are examined in detail for the particular case of iron; and in general to illustrate how the accumulation of pure data will contribute toward the establishment of physiochemical concepts which are required to understand the mechanisms that are operational in friction systems. In the case of iron, LEED, Auger and microcontact studies have established that hydrogen and light-saturated organic vapors do not establish interfaces which prevent iron from welding, whereas oxygen and some oxygen and sulfur compounds do reduce welding as well as the coefficient of friction. Interpretation of these data suggests a mechanism of sulfur interaction in lubricating systems.

Keller, D. V., Jr.↗
NASA NTRS1974

Adsorption and condensation of Cu on W single-crystal surfaces

The adsorption and condensation of Cu up to several monolayers in thickness on tungsten 110 and 100 single-crystal surfaces are studied by combining low-energy electron diffraction, Auger electron spectroscopy, thermal desorption spectroscopy, work-function measurements, and quartz microbalance thickness measurements in one experimental system. The results show drastic differences in the evolution of the structure, work function, and desorption behavior between 110 and 100 surfaces. These differences are understandable in terms of the atomic roughness of the surfaces.

Bauer, E.↗
NASA NTRS1979

Structure and orientation of small particles of platinum deposited on NaCl and mica

The structure of small platinum particles condensed in vacuum onto NaCl (001), NaCl (111) and mica substrates was studied by electron diffraction and electron microscopy. Results show that above a certain substrate temperature decahedral or icosahedral particles are formed. These particles are practically absent with substrates cleaved in high vacuum. They are always much less numerous than in gold films prepared under the same conditions. Assumptions made to explain this phenomenon are: (1) the initial growth of an abnormal structure of the nuclei as opposed by the substrate; (2) the particles disappear before they attain a size which corresponds to the observations; and (3) the particles result from a coalescence mechanism leading to multiple twinned particles.

Renou, A.↗
NASA NTRS1981

Vapor phase diamond growth technology

Ion beam deposition chambers used for carbon film generation were designed and constructed. Features of the developed equipment include: (1) carbon ion energies down to approx. 50 eV; (2) in suit surface monitoring with HEED; (3) provision for flooding the surface with ultraviolet radiation; (4) infrared laser heating of substrate; (5) residual gas monitoring; (6) provision for several source gases, including diborane for doping studies; and (7) growth from either hydrocarbon source gases or from carbon/argon arc sources. Various analytical techniques for characterization of from carbon/argon arc sources. Various analytical techniques for characterization of the ion deposited carbon films used to establish the nature of the chemical bonding and crystallographic structure of the films are discussed. These include: H2204/HN03 etch; resistance measurements; hardness tests; Fourier transform infrared spectroscopy; scanning auger microscopy; electron spectroscopy for chemical analysis; electron diffraction and energy dispersive X-ray analysis; electron energy loss spectroscopy; density measurements; secondary ion mass spectroscopy; high energy electron diffraction; and electron spin resonance. Results of the tests are summarized.

Angus, J. C.↗
NASA NTRS1983

Surfaces

Techniques for the characterization of surface cleanliness and roughness for predicting the quality of an adhesive bond are outlined. Generally, smooth surfaces are only available from cleavage of crystalline materials along a natural cleavage plane. Films must be deposited on metal surfaces to achieve the same smoothness. Once the surfaces are clean, however, reaction with the ambient atmosphere becomes likely through diffusive and absorption processes, producing asperities. Electron diffraction, Auger electron, and X ray emission spectroscopy are used to characterize surface condition. Once the surface is observed to be clean, the application of an adhesive will usually prohibit separation along the adhesive; separation is then confined to the weaker of the two materials. Finally, the use of polytetrafluorothylene adhesive to test the adhesion between polymers and metal surfaces is described.

Buckley, D. H.↗
NASA NTRS1986

Transmission electron microscopic examination of phosphoric acid fuel cell components

Transmission electron microscopy (TEM) was used to physically characterize tested and untested phosphoric acid fuel cell (PAFC) components. Those examined included carbon-supported platinum catalysts, carbon backing paper, and Teflon-bonded catalyst layers at various stages of fabrication and after testing in pressurized PAFC's. Applicability of electron diffraction and electron energy loss spectroscopy for identifying the various phases was explored. The discussion focuses on the morphology and size distribution of platinum, the morphology and structural aspects of Teflon in catalyst layers, and the structural evidence of carbon corrosion. Reference is made to other physical characterization techniques where appropriate. A qualitative model of the catalyst layer that emerged from the TEM studies is presented.

Pebler, A.↗
NASA NTRS2025

Thermochemical Stability of Ca2Yb8(SiO4)6O2 Apatite in Presence of Molten Calcium-Magnesium-AluminoSilicate (CMAS)

Thermochemical stability of ytterbium silicon oxyapatite Ca 2 Yb 8 (SiO 4 ) 6 O 2 (CYbS) in the presence of molten calcium-magnesium aluminosilicate (CMAS) has been investigated at elevated temperatures. CYbS apatite powder was synthesized from the constituent oxides via solid state reaction method. Hot pressed apatite substrates were exposed to molten CMAS at 1200, 1300, and 1400 °C for 1, 10, and 50 h. Development of phases in the interaction region of the heat-treated specimens was monitored using scanning electron microscopy, transmission electron microscopy, high angle annular dark field imaging, selected area electron diffraction and energy dispersive X-ray spectroscopy. Monoclinic cyclosilicate Ca 3 Yb 2 (Si 3 O 9 ) 2 formed from interaction of CYbS apatite with CaO in the CMAS melt at the apatite-CMAS reaction front and continued to nucleate and grow within the residual CMAS in diffusion couples annealed for 1-50 h at 1200 °C and those heat treated at 1300 °C for 1 h. Residual CMAS was Ca-depleted when cyclosilicate was present. Dendritic wollastonite CaSiO 3 was observed within the residual CMAS in couples annealed at 1200 and 1300 °C. Ingress of molten CMAS, because of its exponential decrease in viscosity, occurred through open pores and along the grain boundaries of the apatite substrates without any detectable chemical reaction at 1300 and 1400 °C. Results of this study indicate that Ca 2 Yb 8 (SiO 4 ) 6 O 2 apatite has the potential to mitigate the CMAS corrosion up to about 1200 °C but not at higher temperatures.

X-ray diffraction↗
DOE OSTI2025

Direct structural retrieval from gas-phase ultrafast diffraction data using a genetic algorithm

Ultrafast scattering techniques such as ultrafast electron diffraction and ultrafast x-ray diffraction have been utilized to elucidate the structural dynamics, reaction intermediates, and final products in molecular reactions following photoexcitation. The time-dependent structures are typically not directly retrieved from the experimental data, but they rely on comparison with calculations. The genetic algorithm (GA), a global optimization strategy, can be used to retrieve the molecular structures directly from diffraction patterns without any theoretical input. However, the robustness of the GA with respect to real experimental conditions such as a limited momentum transfer range, noise, and artifacts has not been studied in detail. In this work, we characterize the performance of the GA with simulated data that mimic realistic experimental conditions. We have developed and implemented a variant of the GA specific to diffraction measurements which performs better in the presence of imperfect data compared to the standard implementation of the GA. We demonstrate this method with both synthetic data and experimental ultrafast electron diffraction data on the UV-induced photodissociation of trifluoroiodomethane (C⁢F 3⁡ I) molecules.

74 ATOMIC AND MOLECULAR PHYSICS↗
NASA NTRS1973

Structure of molybdenum disulfide films sputtered on substrates at various temperatures

Molybdenum disulfide films 300 to 400 A thick were rf sputtered on aluminum and nickel surfaces at elevated, ambient, and liquid nitrogen temperatures. Electron transmission micrographs and electron diffraction patterns were taken to determine the structural growth. These transmission micrographs revealed that sputtered MoS2 films at ambient and elevated temperatures (320 and 150 C) formed an irregular network of ridges. The electron diffraction patterns of these films showed relatively sharp diffraction rings, indicating crystallinity. The transmission micrographs of sputtered films at liquid nitrogen temperatures revealed a continuous featureless film. The electron diffraction patterns showed broad, diffused rings indicating an amorphous film. The transmission micrographs of a post-annealed (425 C) MoS2 film sputtered at liquid-nitrogen temperature revealed the tendency for ridge formation. Electron diffraction patterns also showed increased sharpness of the diffraction rings. Friction tests showed that MoS2 films deposited at ambient and elevated temperatures exhibited good lubricating properties. The MoS2 films deposited at cryogenic temperatures had no lubricating characteristics.

Spalvins, T.↗
DOE OSTI2024

Intercalation-Induced Topotactic Phase Transformation of Tungsten Disulfide Crystals

Recent research has demonstrated the potential for topological superconductivity, anisotropic Majorana bound states, optical nonlinearity, and enhanced electrochemical activity for transition metal dichalcogenides (TMDs) with a 2M structure. These unique TMD compounds exhibit metastability and, upon heating, undergo a transition to the thermodynamically stable 2H phase. The 2M phase is commonly made at high temperatures using traditional solid-state methods, and this metastability further complicates the growth of large 2M WS 2 crystals. Herein, a novel synthetic method was developed, focusing on a molten salt reaction to synthesize large 2H crystals and then inducing transformation to the 2M phase through intercalation and thermal treatment. The 2H crystals were intercalated via a room-temperature sodium naphthalenide solution, producing a previously unreported Na-intercalated 2H WS 2 phase. Thermal heating was required to facilitate the phase transition to the intercalated 2M crystal structure. This phase transition was studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), electron dispersive X-ray spectroscopy (EDS), and Raman spectroscopy, which confirmed the synthesis of the intercalated 2M phase. Upon deintercalation, crystal and powder samples showed superconductivity with a T c of 8.6–8.7 K, similar to previously reported values. The generality of this process was further demonstrated using alkali metal triethyl borohydride to intercalate 2H WS 2 and produced the desired 2M phase. This novel synthetic method has broad implications for discovering metastable phases in other TMD families and layered materials. Furthermore, separation of the intercalation and phase transition also has the potential to allow for large-scale synthesis of this technologically important phase with greater control over each step of the reaction.

36 MATERIALS SCIENCE↗
NASA NTRS1995

Transmission electron microscope studies of extraterrestrial materials

Transmission Electron Microscopy, X-Ray spectrometry and electron-energy-loss spectroscopy are used to analyse carbon in interplanetary dust particles. Optical micrographs are shown depicting cross sections of the dust particles embedded in sulphur. Selected-area electron diffraction patterns are shown. Transmission Electron Microscope specimens of lunar soil were prepared using two methods: ion-milling and ultramicrotomy. A combination of high resolution TEM imaging and electron diffraction is used to characterize the opaque assemblages. The opaque assemblages analyzed in this study are dominated by ilmenite with lesser rutile and spinel exsolutions, and traces of Fe metal.

Keller, Lindsay P.↗
DOE OSTI2025

Fast calculation of diffraction patterns from an ensemble of aligned molecules

We report an algorithm to calculate electron diffraction patterns for molecules with anisotropic angular distribution, which is significantly faster than existing methods. The algorithm uses a transform to convert the molecular orientation distribution, which is a function of three Euler angles, to the atom-pair distribution functions which depend on the polar and azimuthal angles. The diffraction signal can then be calculated from the atom-pair distributions. We demonstrate the computation method numerically by calculating electron diffraction patterns for a symmetric top molecule (trifluoroiodomethane) and an asymmetric top molecule (formaldehyde) and show that it reduces the calculation time by approximately two orders of magnitude compared to the standard brute-force method. Here, the method can also be applied to the calculation of x-ray diffraction patterns.

74 ATOMIC AND MOLECULAR PHYSICS↗
NASA NTRS2023

Ceramic Capacitor Grain Size Analysis Using Electron Backscatter Diffraction (EBSD)

The overall scope of this NESC study was to identify (or develop) a tool, methodology, or process that can inspect a ceramic capacitor and consistently return repeatable grain size distribution results. It is important to note that the development of a machine learning technique was considered as an option for this study, but only if an existing automated tool was not available. This report explains why the Electron Backscatter Diffraction analysis method for grain structure and size distribution was deemed a suitable candidate for this work.

Electron Backscatter Diffraction↗
NASA NTRS2009

Electron Backscatter Diffraction (EBSD) Analysis and U-Pb Geochronology of the Oldest Lunar Zircon: Constraining Early Lunar Differentiation and Dating Impact-Related Deformation

The evolution of the early moon was dominated by two processes (i) crystallization of the Lunar Magma Ocean (LMO) and differentiation of potassium-rare earth element-phosphorous-rich residual magma reservoir referred to as KREEP, and (ii) an intense meteorite bombardment referred to as lunar cataclysm . The exact timing of these processes is disputed, and resolution relies on collection and interpretation of precise age data. This study examines the microstructure and geochronology of zircon from lunar impact breccias collected during the Apollo 17 mission. A large zircon clast within lunar breccia 72215,195 shows sector zoning in optical microscopy, cathodoluminescence (CL) imaging and Raman mapping, and indicates that it was a relict fragment of a much larger magmatic grain. Sensitive high resolution ion microprobe (SHRIMP) U-Pb analysis of the zircon shows that U and Th concentration correlate with sector zoning, with darkest CL domains corresponding with high-U and Th (approx.150 and approx.100 ppm respectively), and the brightest-CL sectors containing approx.30-50 ppm U and approx.10-20 ppm Th. This indicates that variations in optical CL and Raman properties correspond to differential accumulation of alpha-radiation damage in each sector. Electron backscatter diffraction (EBSD) mapping shows that the quality of electron backscatter patterns (band contrast) varies with sector zoning, with the poorest quality patterns obtained from high-U and Th, dark-CL zones. EBSD mapping also reveals a deformation microstructure that is cryptic in optical, CL and Raman imaging. Two orthogonal sets of straight discrete and gradational low-angle boundaries accommodate approx.12 misorientation across the grain. The deformation bands are parallel to the crystallographic {a}-planes of the zircon, have misorientation axes parallel to the c-axis, and are geometrically consistent with formation by dislocation creep associated with <100>{010} slip. The deformation bands are unlike curved morphology of crystal-plastic microstructures in tectonically deformed terrestrial zircon, and geometrically similar to dislocation microstructures reported in experimentally shocked zircon. We interpret these crystal-plastic deformation microstructures to have resulted from a significant impact, either directly from impact shock, or during ductile flow directly following the impact. The deformation bands appear to continue undeflected through the non-indexed, radiation-damaged areas of the grain, which suggests that the orientation variation predates any significant mechanical weakening from radiation damage in the grain, and therefore occurred early in its history.

Timms, Nick↗