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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 1,189 records · Page 66
All sourcesNASA NTRSDOE OSTI
NASA NTRS1992

Spatiotemporal chaos near the onset of cellular growth during thin-film solidification of a binary alloy

Thin-film solidification experiments with a succinonitrile-acetone alloy are used to observe the long time-scale dynamics of cellular crystal growth at growth rates only slightly above the critical value VC = Vc(lambda sub c) for the onset of morphological instability. Under these conditions only very small amplitude cells are observed with wavelengths near the value predicted by linear stability theory lambda = lambda sub c. At long times, microstructures with wavelengths significantly finer than lambda suc c form by nucleation at defects across the interface. These interfaces do not have a unique microstructure, but seem to exhibit spatiotemporal chaos on a long time scale caused by the continual birth and death of cells by tip splitting and cell annihilation in grooves.

Lee, J. T. C.↗
NASA NTRS1995

The Metastable Persistence of Vapor-Deposited Amorphous Ice at Anomalously High Temperatures

Studies of the gas release, vaporization behavior and infrared (IR) spectral properties of amorphous and crystalline water ice have direct application to cometary and planetary outgassing phenomena and contribute to an understanding of the physical properties of astrophysical ices. Several investigators report anomalous phenomena related to the warming of vapor-deposited astrophysical ice analogs. However gas release, ice volatilization and IR spectral features are secondary or tertiary manifestations of ice structure or morphology. These observations are useful in mimicking the bulk physical and chemical phenomena taking place in cometary and other extraterrestrial ices but do not directly reveal the structural changes which are their root cause. The phenomenological interpretation of spectral and gas release data is probably the cause of somewhat contradictory explanations invoked to account for differences in water ice behavior in similar temperature regimes. It is the microstructure, micromorphology and microchemical heterogeneity of astrophysical ices which must be characterized if the mechanisms underlying the observed phenomena are to be understood. We have been using a modified Transmission Electron Microscope to characterize the structure of vapor-deposited astrophysical ice analogs as a function of their deposition, temperature history and composition. For the present experiments, pure water vapor is deposited at high vacuum onto a 15 K amorphous carbon film inside an Hitachi H-500H TEM. The resulting ice film (approx. 0.05 micrometers thick) is warmed at the rate of 1 K per minute and diffraction patterns are collected at 1 K intervals. These patterns are converted into radial intensity distributions which are calibrated using patterns of crystalline gold deposited on a small part of the carbon substrate. The small intensity contributed by the amorphous substrate is removed by background subtraction. The proportions of amorphous and crystalline material in each pattern are determined by subtracting a percentage of crystalline component relative to amorphous and pure crystalline endmembers. Vapor-deposited water ice undergoes two amorphous to amorphous structural transformations in the temperature range 15-130 K with important astrophysical implications. The onset of cubic crystallization occurs at 142-160 K (at 1K per minute heating rates) during which the 220 and 311 diffraction maxima appear and 0.1 micrometer crystallites can be seen in bright field images. This transition is time dependent.

Blake, David F.↗
DOE OSTI2016

Linking microstructural evolution and macro-scale friction behavior in metals [Predicting the friction behavior of metals using a microstructural evolution model]

A correlation is established between the macro-scale friction regimes of metals and a transition between two dominant atomistic mechanisms of deformation. Metals tend to exhibit bi-stable friction behavior—low and converging or high and diverging. These general trends in behavior are shown to be largely explained using a simplified model based on grain size evolution, as a function of contact stress and temperature, and are demonstrated for self-mated pure copper and gold sliding contacts. Specifically, the low-friction regime (where µ < 0.5) is linked to the formation of ultra-nanocrystalline surface films (10–20 nm), driving toward shear accommodation by grain boundary sliding. Above a critical combination of stress and temperature—demonstrated to be a material property—shear accommodation transitions to dislocation dominated plasticity and high friction, with µ > 0.5. We utilize a combination of experimental and computational methods to develop and validate the proposed structure–property relationship. As a result, this quantitative framework provides a shift from phenomenological to mechanistic and predictive fundamental understanding of friction for crystalline materials, including engineering alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Development and Understanding of Nb 3 Sn films for radiofrequency applications through a sample-host 9-cell cavity

Nb 3 Sn is a promising advanced material under development for superconducting radiofrequency cavities. Past efforts have been focused primarily on small development-scale cavities, but large, often multi-celled cavities, are needed for particle accelerator applications. In this work, we report on successful Nb 3 Sn coatings on Nb in a 1 m-long 9-cell Nb sample-host cavity at Fermilab. The geometry of the first coating with only one Sn source made it possible to study the influence of Sn flux on the microstructure. Based on these results, we postulate a connection between recently observed anomalously large thin grains and uncovered niobium spots observed in the past by other authors (Trenikhina et al 2018 Supercond. Sci. Technol. 32 015004). A phenomenological model to explain how these anomalously large grains could form is proposed. Overall, this model is invoked to provide possible explanations for literature results from several groups and to guide key process parameters to achieve uniform vapor-diffusion coatings, when applied to complex structures as the multi-cell cavity under study.

43 PARTICLE ACCELERATORS↗
DOE OSTI2024

Multilaminate Energy Storage Films from Entropy‐Driven Self‐Assembled Supramolecular Nanocomposites

Abstract Composite materials comprising polymers and inorganic nanoparticles (NPs) are promising for energy storage applications, though challenges in controlling NP dispersion often result in performance bottlenecks. Realizing nanocomposites with controlled NP locations and distributions within polymer microdomains is highly desirable for improving energy storage capabilities but is a persistent challenge, impeding the in‐depth understanding of the structure–performance relationship. In this study, a facile entropy‐driven self‐assembly approach is employed to fabricate block copolymer‐based supramolecular nanocomposite films with highly ordered lamellar structures, which are then used in electrostatic film capacitors. The oriented interfacial barriers and well‐distributed inorganic NPs within the self‐assembled multilaminate nanocomposites effectively suppress leakage current and mitigate the risk of breakdown, showing superior dielectric strength compared to their disordered counterparts. Consequently, the lamellar nanocomposite films with optimized composition exhibit high energy efficiency (>90% at 650 MV m −1 ), along with remarkable energy density and power density. Moreover, finite element simulations and statistical modeling have provided theoretical insights into the impact of the lamellar structure on electrical conduction, electric field distribution, and electrical tree propagation. This work marks a significant advancement in the design of organic–inorganic hybrids for energy storage, establishing a well‐defined correlation between microstructure and performance.

Li, He↗
DOE OSTI2024

Interdependence of Support Wettability - Electrodeposition Rate- Sodium Metal Anode and SEI Microstructure

Here, this study examines how current collector support chemistry (sodiophilic intermetallic Na 2 Te vs. sodiophobic baseline Cu) and electrodeposition rate affect microstructure of sodium metal and its solid electrolyte interphase (SEI). Capacity and current (6 mAh cm -2 , 0.5–3 mA cm -2 ) representative of commercially relevant mass loading in anode-free sodium metal battery (AF-SMBs) are analyzed. Synchrotron X-ray nanotomography and grazing-incidence wide-angle X-ray scattering (GIWAXS) are combined with cryogenic ion beam (cryo-FIB) microscopy. Highlighted are major differences in film morphology, internal porosity, and crystallographic preferred orientation e.g. (110) vs. (100) and (211) with support and deposition rate. Within the SEI, sodium fluoride (NaF) is more prevalent with Te-Cu versus sodium hydride (NaH) and sodium hydroxide (NaOH) with baseline Cu. Due to competitive grain growth the preferred orientation of sodium crystallites depends on film thickness. Mesoscale modeling delineates the role of SEI (ionic conductivity, morphology) on electrodeposit growth and onset of electrochemical instability.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Toward Optimizing Electrospun Nanofiber Fuel Cell Catalyst Layers: Microstructure and Pt Accessibility

This work investigates how local ionomer/platinum (Pt) interactions and ionomer distribution in electrospun Pt/Vulcan nanofiber electrodes impact ionomer coverage, proton accessibility, and oxygen reduction reaction (ORR) performance in proton-exchange membrane fuel cells. Insights from various in situ electrochemical diagnostics were utilized in conjunction with ex situ microscopic characterization to understand how the electrode microstructure—both at the aggregate level and near the ionomer/platinum interface—is affected by electrospinning in comparison to ultrasonic spraying. The effect of the carrier polymer poly(acrylic acid) (PAA) concentration from 5–20 wt % (with respect to total ink solids) on the resulting nanofiber morphology is discussed. Electron microscopy observations and CO displacement measurements indicated that Pt/Vulcan nanofibers prepared with a higher PAA concentration (15 wt %) were conformally coated with a film of ionomer on the exterior of the fiber, which resulted in an overall lower ionomer coverage on both Pt and carbon throughout the fiber diameter. In contrast, 10 wt % PAA leads to a uniform intrafiber distribution of the ionomer within the fibers, increasing the overall ionomer coverage and proton accessibility under both wet and dry conditions. These differences in the local ionomer coverage on Pt between 10 and 15 wt % PAA were also attributed to differences in the adsorption/interaction affinities between PAA and the ionomer onto the catalyst surface in the ink using zeta potential measurements. Additional fuel cell electrochemical tests on the electrospun electrodes show improvements in ORR kinetics and high-current-density H 2 /air performance compared to the ultrasonically sprayed electrodes.

25 ENERGY STORAGE↗
NASA NTRS1986

On the determination of the origin of linear anomaly in the macrostructure of VPPA welded 2219-T87 aluminum alloy

The objective was to determine the cause and significance of the weld radiograph enigma, which is a linear anomaly in the features of the X-ray film. By observing features on available radiographs and in studying published reports of similar features it was possible to conclude that there are many manifestations of the enigma, and that they are all specific features of fine structure in radiographs due to natural processes connected with welding and to specific X-ray absorption and diffraction phenomena. These processes include the thermal distribution and liquid metal flow in welding, the development of microstructure, morpohology, second phase particles and porosity due to the solidification process and to the pattern of residual stresses after the weld metal has cooled to the ambient temperature. Microdensitometer traces were made across weld radiographs of standard and enigmatic types. Similar patterns were produced by computer simulation. These show that the enigma is a relatively low contrast feature compared to real weld defects, such as undercuts or centerline cracks. The enigma can be distinguished from weld defects by these microdensitometer traces. The enigma effect on weld properties is not known but is expected to be minor.

Jemian, W. A.↗
DOE OSTI2016

Recent Advances in Analytical Electron Microscopy for Irradiated Materials

Analytical electron microscopy (AEM) in the scanning transmission electron microscope (STEM) has long been a staple of post-irradiation examination (PIE) and materials development campaigns. Recently, new advances in both STEM hardware and post-processing data-analysis software, along with ancillary advances such as in focused ion beam (FIB) sample preparation, has led to exciting advances in the quantity and quality of data that can be obtained. This talk will summarize recent experiments performed at Oak Ridge National Laboratory (ORNL), especially work on neutron-irradiated materials and fuels taking advantage of a newly-installed latest-generation AEM tool in the ORNL irradiated materials laboratories. ORNL installed a new FEI Talos F200X microscope, a 200 keV, high-brightness Schottky emission AEM system optimized for high-speed, high-efficiency X-ray mapping experiments. The F200X features the FEI 'SuperX' four-sector silicon drift detector (SDD) X-ray detector, which provides 0.9 sr solid angle of collection. By combining the high-brightness electron source, latest-generation electron optics, and fast computers and pulse processors, X-ray mapping speed is increased by a factor of 50-100 x compared to the previous-generation instruments. In addition to improvements in hardware, data mining via multivariate statistical analysis (MVSA) allows for maximum insight to the data obtained from the new hardware. MVSA data mining of the X-ray maps allows, for instance, unbiased computational identification of the phases present, and discovery of small phases or precipitates not expected by the human analyst. This talk will present examples of experiments performed using the most modern AEM tools and software. Silicon carbide is a major candidate for next-generation nuclear applications. Nano-infiltration by transient eutectic (NITE) SiC requires low sintering temperatures. X-ray mapping of the NITE structure find pockets of different oxides, such as Zr-Y-oxide, Y-Al-oxide, and yttria. MVSA data mining finds the regions where different oxides are present and indicates that Y additions preferentially wet grain boundaries, where Zr additions are preferentially concentrated at grain triple points. SiC coatings from AGR-I experiment TRISO particles were found to contain significant quantities of fission products (e.g., Pd) as well as actinides (U, Pu). MVSA data mining found complex precipitates and grain boundary films of the fission products and actinides deep (∼several microns) into the SiC layer. Advanced AEM methods, combined with MVSA data mining, makes possible both rapid and detailed PIE. Ferritic alloys, such as accident-tolerant FeCrAl grades, benefit greatly from advanced AEM examination. Neutron-irradiated FeCrAl precipitates the detrimental Cr-rich α' phase. Because the SuperX SDD system has four detectors, it is possible to obtain high X-ray count rates even on a highly tilted specimen, as might be needed to obtain STEM images of dislocation loops. Results on neutron-irradiated FeCrAl indicates that α' size and number density can be obtained by AEM, and MVSA results determine that minor elements (such as Si) has complex radiation-induced segregation behavior at grain boundaries. We have also developed and validated computer models of the AEM experiment, allowing different microstructures' X-ray map results to be simulated for different STEM instruments. This allows X-ray mapping to be more quantitative, such as by estimating what size nanoclusters in an oxide-dispersion strengthened steel would be visible or invisible in STEM. In summary, new advanced AEM technology provides a major leap forward in experiments possible in PIE of irradiated materials. (authors)

36 MATERIALS SCIENCE↗
DOE OSTI2019

THz emission from Co/Pt bilayers with varied roughness, crystal structure, and interface intermixing

Ultrafast demagnetization of Co/Pt heterostructures induced by a femtosecond 800-nm laser pulse launches a spin current from Co to Pt and subsequent conversion of the spin current to a charge current in the Pt layer due to the inverse spin-Hall effect. At the same time, due to the spin-dependent photogalvanic effect, a circularly polarized femtosecond laser pulse also generates a photocurrent at the Co/Pt interface. Both ultrashort photocurrent pulses are effectively detected in a contactless way by measuring the THz radiation they emit. Here we aim to understand how the properties of the Co/Pt interface affect the photocurrents in the bilayers. By varying the interfacial roughness, crystal structure, and interfacial intermixing, as well as having an explicit focus on the cases when THz emissions from these two photocurrents reveal opposite trends, we identify which interface properties play a crucial role for the photocurrents. In particular, we show that by reducing the roughness, the THz emission due to the spin-dependent photogalvanic effect reduces to zero while the strength of the THz emission from the photocurrent associated with the inverse spin-Hall effect increases by a factor of 2. On the other hand, while intermixing strongly enhances the THz emission from the inverse spin-Hall effect by a factor of 4.2, THz emission related to the spin-dependent photogalvanic effect reveals the opposite trend. Furthermore, these findings indicate that microstructural properties of the Co-Pt interface play a decisive role in the generation of photocurrents.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Study on Interfacial Phenomena in Aluminum–Aluminum Bimetal Fabricated by Extrusion at Different Temperatures

Aluminum–aluminum bimetal was prepared by spray-formed Al22Si alloy and ZL102 through extrusion process under solid–solid state, semisolid state and solid–liquid state. The microstructures and bonding strength of the bimetallic interface were studied, and the fracture behaviors of different bimetallic states were compared. The results showed that perfect metallic bond is produced through the semisolid extrusion process. The bimetal through solid–solid extrusion process is a large number of particles extruding through gaps among the cracked oxide layers, thus realized the metallurgical combination with the virgin metal. The process of semisolid extrusion is to break the oxide film under the temperature and pressure to achieve the bimetallic bonding. Besides, the hard particles wrapped by liquid metal can also enhance bonding strength. The tensile strength of bimetal fabricated by semisolid extrusion shows more promising results than that made by solid–solid combination and solid–liquid combination; the tensile strength improved from 83.3 to 120.5 MPa, an increase of about 45%. The process presented in this study provides a promising and effective approach for achieving Al22Si/Zl102 bimetal with high-quality metallurgical bonded interface.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Nucleation-promoting and growth-limiting synthesis of disordered rock-salt Li-ion cathode materials

Disordered rock-salt oxides and oxyfluorides are promising positive electrode materials for high-performance lithium-ion batteries free of nickel and cobalt. However, conventional synthesis methods rely on post-synthesis pulverization to achieve cycling-appropriate particle sizes, offering limited control over particle microstructure and crystallinity. This accelerates degradation and complicates secondary particle processing. Here we present a synthesis strategy that enhances nucleation while suppressing particle growth and agglomeration across various disordered rock-salt compositions, including lithium–manganese–titanium oxide, lithium–manganese–niobium oxide, and lithium–nickel–titanium oxide systems. Applied to Li 1.2 Mn 0.4 Ti 0.4 O 2 , this method yields highly crystalline, well-dispersed sub-200 nm particles that form homogeneous electrode films with stable cycling behavior. Tested in cells with lithium metal as the counter electrode, these electrodes deliver ~200 mAh/g with 85% capacity retention relative to the first cycle after 100 cycles (20 mA/g, 1.5–4.8 V), and an average discharge voltage loss of 4.8 mV per cycle, compared to 38.6% retention and 7.5 mV loss per cycle for electrodes derived from pulverized solid-state particles. This approach suggests a route to enhance the performance and durability of disordered rock-salt electrodes for sustainable lithium-ion batteries.

Batteries↗
NASA NTRS1986

On the determination of the origin of linear anomaly in the macrostructure of VPPA welded 2219-T87 aluminum alloy: Preliminary report

The cause and significance of the weld radiograph enigma, which is a linear anomaly in the features of the X-ray film is examined. By observing features on available radiographs and in studying published reports of similar features, it was possible to conclude that there are many manifestations of the enigma, and that they are all specific features of fine structure in radiographs due to natural processes connected with welding and to specific X-ray absorption and diffraction phenomena. These processes include the thermal distribution and liquid metal flow in welding, the development of microstructure, morphology, second phase particles and porosity due to the solidification process, and to the pattern of residual stresses after the weld metal has cooled to the ambient temperature. Microdensitometer traces were made across weld radiographs of standard enigmatic types. Similar patterns were produced by computer simulation. These show that the enigma is a relatively low contrast feature compared to real weld defects, such as undercuts or centerline cracks. The enigma can be distinguished from weld defects by these microdensitometer traces. The enigma effect on weld properties is not known but is expected to be minor.

Jemian, W. A.↗
DOE OSTI2023

Revealing Possible Coherence Limiting Sources in Superconducting Qubit with Advanced Electron Microscopy

Superconducting materials hold great potential for solid-state quantum computing. Their fabrication relies on established semiconductor fabrication techniques, such as thin film deposition and lithography, but the complex processing steps can result in defects at the qubits' interfaces and surfaces that can negatively impact coherence time. To improve superconducting qubit performance, it is essential to understand the structural features, at the atomic scale, that may act as sources of decoherence limiting factor in both the Josephson junction (JJ) and resonators, which are key components of superconducting qubit. This talk will present our recent studies on the microstructures in a 2D-transmon, with an emphasis on the JJ. For this research, a combination of advanced microscopy techniques, including high-resolution (S)TEM imaging, and spectroscopy (EDS and EELS) are used to identify possible coherence-limiting defects or structural features.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Change in equilibrium position of misfit dislocations at the GaN/sapphire interface by Si-ion implantation into sapphire—I. Microstructural characterization

Much research has been done to reduce dislocation densities for the growth of GaN on sapphire, but has paid little attention to the elastic behavior at the GaN/sapphire interface. In this study, we have examined effects of the addition of Si to a sapphire substrate on its elastic property and on the growth of GaN deposit. Si atoms are added to a c-plane sapphire substrate by ion implantation. The ion implantation results in scratches on the surface, and concomitantly, inhomogeneous distribution of Si. The scratch regions contain a higher concentration of Si than other regions of the sapphire substrate surface, high-temperature GaN being poorly grown there. However, high-temperature GaN is normally grown in the other regions. The GaN overlayer in the normally-grown regions is observed to have a lower TD density than the deposit on the bare sapphire substrate (with no Si accommodated). As compared with the film on an untreated, bare sapphire, the cathodoluminescence defect density decreases by 60 % for the GaN layer normally deposited on the Si-ion implanted sapphire. As confirmed by a strain mapping technique by transmission electron microscopy (geometric phase analysis), the addition of Si in the normally deposited regions forms a surface layer in the sapphire elastically more compliant than the GaN overlayer. The results suggest that the layer can largely absorb the misfit strain at the interface, which produces the overlayer with a lower defect density. Our results highlight a direct correlation between threading-dislocation density in GaN deposits and the elastic behavior at the GaN/sapphire interface, opening up a new pathway to reduce threading-dislocation density in GaN deposits.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Single and multi-layered core-shell structures based on ZnO nanorods obtained by aerosol assisted chemical vapor deposition

Core–shell nanorod structures were prepared by a sequential synthesis using an aerosol assisted chemical vapor deposition technique. Several samples consisting of ZnO nanorods were initially grown over TiO{sub 2} film-coated borosilicate glass substrates, following the synthesis conditions reported elsewhere. Later on, a uniform layer consisting of individual Al, Ni, Ti or Fe oxides was grown onto ZnO nanorod samples forming the so-called single MO{sub x}/ZnO nanorod core–shell structures, where MO{sub x} was the metal oxide shell. Additionally, a three-layer core–shell sample was developed by growing Fe, Ti and Fe oxides alternately, onto the ZnO nanorods. The microstructure of the core–shell materials was characterized by grazing incidence X-ray diffraction, scanning and transmission electron microscopy. Energy dispersive X-ray spectroscopy was employed to corroborate the formation of different metal oxides. X-ray diffraction outcomes for single core–shell structures showed solely the presence of ZnO as wurtzite and TiO{sub 2} as anatase. For the multi-layered shell sample, the existence of Fe{sub 2}O{sub 3} as hematite was also detected. Morphological observations suggested the existence of an outer material grown onto the nanorods and further microstructural analysis by HR-STEM confirmed the development of core–shell structures in all cases. These studies also showed that the individual Al, Fe, Ni and Ti oxide layers are amorphous; an observation that matched with X-ray diffraction analysis where no apparent extra oxides were detected. For the multi-layered sample, the development of a shell consisting of three different oxide layers onto the nanorods was found. Overall results showed that no alteration in the primary ZnO core was produced during the growth of the shells, indicating that the deposition technique used herein was and it is suitable for the synthesis of homogeneous and complex nanomaterials high in quality and purity. In addition, materials absorptance determined from the total transmittance and reflectance spectra revealed a broader absorption interval including visible light, indicating potential uses of these nanostructures on solar energy appliances. - Graphical abstract: Display Omitted - Highlights: • Uniform ZnO nanorods (core)–metal oxide (shell) were obtained sequentially by AACVD. • Shells were structured of homogeneous single or multi-layered non-mixed metal oxides. • ZnO nanorod core was preserved during the shell synthesis. • Optical absorptance revealed visible interval absorption for FeO{sub x} shell samples. • Materials can be suitable for photocatalytic or photovoltaic applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Oxide Morphology of C26M at 300 - 600 °C

Iron-chromium-aluminum (FeCrAl) alloys are of interest to the nuclear materials community due to their resistance to high temperature steam oxidation under accident conditions. The present work investigates oxide formation at temperatures relevant to light water reactor cladding operation following extended aging to assess growth kinetics, chemical composition, and microstructure of oxide formation on an Oak Ridge National Laboratory developed Fe-12Cr-6Al- 2Mo-0.2Si-0.03Y alloy (designated ‘C26M’). Aging treatments were performed for 100-2000 hours in stagnant air at 300, 400, 500, and 600 °C, respectively. Oxide growth behavior under the investigated conditions follows a logarithmic time dependence. When the oxidization temperature is 400 °C or below, the oxide is amorphous. At 500 °C, crystalline α-Al 2 O 3 oxide film develops and the correlated logarithmic rate constant decreases significantly, indicating enhanced oxidation resistance of the formed oxide film. In addition, Mo segregation at grain boundaries has been observed when the aging temperature exceeds 500 °C. The results of this study can be viewed as an upper bounding result for potential oxide coarsening on the cladding inner surface during reactor operation.

36 MATERIALS SCIENCE↗