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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 685 records · Page 38
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Solidification and crystallographic texture modeling of laser powder bed fusion Ti-6Al-4V using finite difference-monte carlo method

Laser powder bed fusion (LPBF) additive manufacturing makes near-net-shaped parts with reduced material cost and time, rising as a promising technology to fabricate Ti-6Al-4V, a widely used titanium alloy in aerospace and medical industries. However, LPBF Ti-6Al-4V parts produced with 67° rotation between layers, a scan strategy commonly used to reduce microstructure and property inhomogeneity, have varying grain morphologies and weak crystallographic textures that change depending on processing parameters. Here, this study predicts LPBF Ti-6Al-4V solidification at three energy levels using a finite difference-Monte Carlo method and validates the simulations with large-area electron backscatter diffraction (EBSD) scans. The developed model accurately shows that a <001> texture forms at low energy and a <111> texture occurs at higher energies parallel to the build direction but with a lower strength than the textures observed from EBSD. A validated and well-established method of combining spatial correlation and general spherical harmonics representation of texture is developed to calculate a difference score between simulations and experiments. The quantitative comparison enables effective fine-tuning of nucleation density (N 0 ) input, which shows a nonlinear relationship with increasing energy level. Future improvements in texture prediction code and a more comprehensive study of N 0 with different energy levels will further advance the optimization of LPBF Ti-6Al-4V components. These developments contribute a novel understanding of crystallographic texture formation in LPBF Ti-6Al-4V, the development of robust model validation and calibration pipeline methodologies, and provide a platform for mechanical property prediction and process parameter optimization.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2023

Engineering of Nanoscale Heterogeneous Transition Metal Dichalcogenide–Au Interfaces

Engineering the transition metal dichalcogenide (TMD)–metal interface is critical for the development of two-dimensional semiconductor devices. By directly probing the electronic structures of WS 2 –Au and WSe 2 –Au interfaces with high spatial resolution, we delineate nanoscale heterogeneities in the composite systems that give rise to local Schottky barrier height modulations. Photoelectron spectroscopy reveals large variations (>100 meV) in TMD work function and binding energies for the occupied electronic states. Characterization of the composite systems with electron backscatter diffraction and scanning tunneling microscopy leads us to attribute these heterogeneities to differing crystallite orientations in the Au contact, suggesting an inherent role of the metal microstructure in contact formation. Here we then leverage our understanding to develop straightforward Au processing techniques to form TMD–Au interfaces with reduced heterogeneity. Our findings illustrate the sensitivity of TMDs’ electronic properties to metal contact microstructure and the viability of tuning the interface through contact engineering.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Fermi surface of the flat-band intermetallics A P d 3 ( A = Pb , Sn )

The intermetallic phases APd 3 (A = Pb, Sn) were recently predicted to host an unconventional combination of unique electronic structure features, namely, flat bands near the Fermi energy coexisting with topologically protected surface states at the Gamma point. These features each could independently produce alternative electronic states, including electronically or magnetically ordered states coexisting with unconventional edge dominated transport and a significantly large thermopower coexisting with topological characteristics. To explore these expectations, we report the synthesis, structural/chemical characterization, electrical and thermal transport properties, magnetic torque (up to 45 T), and Fermi surface mapping for single crystals produced using the Czochralski technique. X-ray diffraction and scanning transmission electron microscope measurements establish the absence of defects, while small measured values of the thermopower indicate that the Fermi level is located away from the flat-band region. The electronic properties are further clarified by the topography of the Fermi surfaces, measured through the de Haas–van Alphen effect. We find that the Fermi levels are placed at higher energy values than the original ones resulting from the density functional theory calculations, 54 meV higher for PbPd 3 and 68 meV higher for SnPd 3 . Furthermore, the molten flux method was used to synthesize PbPd 3 , yielding nearly identical Fermi surfaces between the specimens grown using different synthesis techniques, indicating the robustness of the Fermi level position. According to the density functional theory calculations, the flat band is mainly formed by the 4d bands of Pd. Thus, we propose monovalent doping on the Pb/Sn site as a viable approach to accessing the flat band while maintaining the unique band structure features of these compounds.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Microstructural Development and Mechanical Properties of Friction Stir Welded Ferritic Stainless Steel AISI 409

This work investigates the effect of friction stir welding process parameters (rotation rate and traverse speed) on the microstructural evolution of friction stir welded (FSWed) ferritic stainless steel (FSS) AISI 409. Optical microscope, scanning electron microscope and electron backscattering diffraction are used to quantitatively assess the development in grain structure and texture. The microstructural development suggested that thermo-mechanical deformation occurs in the stir zone within the austenite/ferrite phase region, ultimately transforming upon cooling into bainitic/ferritic microstructure. The fraction and size of the bainitic/ferritic grains are found to vary through the thickness of the joints. High fractions of coarse ferritic grains are found near the top of the stir zone, and low fraction of fine ferritic grains is found near the bottom of the stir zone. This bainitic/ferritic grain structure resulted in an increase in the hardness of the stir zone by about 74% relative to the base material. The tensile strength of the FSWed FSS joints is almost at the same level of the base material with reduction in the ductility as a result of the increased hardness of the weld zone.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Quantifying Equiaxed vs Epitaxial Solidification in Laser Melting of CMSX-4 Single Crystal Superalloy

The competition between epitaxial vs. equiaxed solidification has been investigated in CMSX-4 single crystal superalloy during laser melting as practiced in additive manufacturing. Single-track laser scans were performed on a powder-free surface of directionally solidified CMSX-4 alloy with several combinations of laser power and scanning velocity. Electron backscattered diffraction (EBSD) mapping facilitated identification of new orientations, i.e., “stray grains” that nucleated within the fusion zone along with their area fraction and spatial distribution. Using high-fidelity computational fluid dynamics simulations, both the temperature and fluid velocity fields within the melt pool were estimated. This information was combined with a nucleation model to determine locations where nucleation has the highest probability to occur in melt pools. In conformance with general experience in metals additive manufacturing, the as-solidified microstructure of the laser-melted tracks is dominated by epitaxial grain growth; nevertheless, stray grains were evident in elongated melt pools. It was found that, though a higher laser scanning velocity and lower power are generally helpful in the reduction of stray grains, the combination of a stable keyhole and minimal fluid velocity further mitigates stray grains in laser single tracks.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Squeezing clathrate cages to host trivalent rare-earth guests

Strike difference of the trivalent rare-earth cations from their alkali and alkaline-earth peers is in the presence of localized 4f-electrons and strong spin-orbit coupling. Placing trivalent rare-earth cations inside the fullerene molecules or in between the blocks of itinerant magnetic intermetallics gave rise to plethora of fascinating properties and materials. A long-time missing but hardly desired piece is the semiconducting or metallic compound where rare-earth cations are situated inside the oversized polyhedral cages of three-dimensional framework. In this work we present a synthesis of such compounds, rare-earth containing clathrates Ba 8-x R x Cu 16 P 30 . The unambiguous proofs of their composition and crystal structure were achieved by a combination of synchrotron powder diffraction, time-of-flight neutron powder diffraction, scanning-transmission electron microscopy, and electron energy-loss spectroscopy. Our quantum-mechanical calculations and experimental characterizations show that the incorporation of the rare-earth cations significantly enhances the hole mobility and concentration which results in the drastic increase in the thermoelectric performance.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Designing Ta C Virtual Substrates for Vertical Al x Ga 1 − x N Power Electronics Devices

Power electronics are critical for a sustainable energy future, playing a key role in electrification and integration of renewable energy sources into the grid. Advances in ultrawide band gap materials are needed to handle higher powers in smaller form factors while reducing electrical and thermal losses. High Al content Al x Ga 1 − x N is theoretically capable of meeting these demands, but its impact in power electronics has been severely restricted by a lack of substrates that can satisfy conductivity, lattice matching, and/or thermal expansion requirements. We demonstrate that electrically conductive Ta C can be used as a virtual substrate for Al x Ga 1 − x N heteroepitaxy. Scaleably sputtered Ta C grown on Al 2 O 3 , followed by high-temperature face-to-face annealing, produces a thin film Ta C template with an effective hexagonal lattice constant matched to Al 0.70 Ga 0.30 N . Annealing of the Ta C promotes recrystallization, significantly improving crystallinity and reducing crystalline defects from as-deposited columnar grains to a step-and-terrace surface morphology, enabling the subsequent growth of high-quality Al 0.70 Ga 0.30 N by molecular beam epitaxy. X-ray diffraction and scanning transmission electron microscopy confirm that the Al x Ga 1 − x N layer is heteroepitaxially aligned, strain-free, and lattice-matched, transitioning abruptly from Ta C to Al x Ga 1 − x N without intermediate phases. These results demonstrate Ta C virtual substrates as electrically conductive, lattice-matched, and thermally compatible templates for vertical Al x Ga 1 − x N devices that can meet the growing power needs of a sustainable energy future. Published by the American Physical Society 2024

36 MATERIALS SCIENCE↗
NASA NTRS1990

Silicon carbon alloy thin film depositions using electron cyclotron resonance microwave plasmas

Amorphous and microcrystalline silicon carbon films (a-SiC:H, micro-c-SiC:H) have been deposited using SiH4, CH4 and H2 mixed gas ECR (electron cyclotron resonance) plasmas. The optical bandgap of a-SiC:H films is not dependent on the hydrogen dilution in the ECR plasma. The deposition rate of a-SiC:H films is found to be strongly dependent on the ECR magnetic field and the hydrogen dilution. The hydrogen dilution effect on the deposition rate indicates that the etching in ECR hydrogen plasmas plays an important role in the deposition of a-SiC:H films. The optical constants n and k of ECR-deposited a-SiC:H films in the wavelength region of 0.4 to 1.0 micron are determined to be 2.03-1.90 and 0.04-0.00, respectively. The microstructures of ECR-deposited micro-c-SiC:H films are shown by X-ray diffraction and SEM (scanning electron microscopy) to be composed of 1000-A alpha-SiC microcrystallites and amorphous network structures.

Shing, Y. H.↗
DOE OSTI2016

Quantification of retained austenite by X-ray diffraction and saturation magnetization in a supermartensitic stainless steel

The good performance of supermartensitic stainless steels is strongly dependent on the volume fraction of retained austenite at room temperature. The present work investigates the effect of secondary tempering temperatures on this phase transformation and quantifies the amount of retained austenite by X-ray diffraction and saturation magnetization. The steel samples were tempered for 1 h within a temperature range of 600–800 °C. The microstructure was characterized using scanning electron microscopy and electron backscatter diffraction. Results show that the amount of retained austenite decreased with increasing secondary tempering temperature in both quantification methods. - Highlights: • The phase transformation during secondary tempering temperatures was observed. • Phases were quantified by X-ray diffraction and DC-saturation magnetization. • More retained austenite forms with increasing secondary tempering temperature. • The retained austenite is mainly located at the grain and lath boundaries.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructural changes and strain hardening effects in abrasive contacts at different relative velocities and temperatures

Strain hardening is commonly used to reach the full potential of materials and can be beneficial in tribological contacts. 2-body abrasive wear was simulated in a scratch test, aimed at strain hardening effects in various steels. Different working conditions were examined at various temperatures and velocities. Strain hardening effects and microstructural changes were analysed with high resolution scanning electron microscopy (HRSEM), electron backscatter diffraction (EBSD), micro hardness measurements and nanoindentation. Statistical analysing was performed quantifying the influence of different parameters on microstructures. Results show a crucial influence of temperature and velocity on the strain hardening in tribological contacts. Increased velocity leads to higher deformed microstructures and higher increased surface hardness at a lower depth of the deformed zones at all materials investigated. An optimised surface hardness can be achieved knowing the influence of velocity (strain rate) and temperature for a “tailor-made” surface hardening in tribological systems aimed at increased wear resistance. - Highlights: •Hardening mechanisms and their intensity in tribological contacts are dependent on relative velocity and temperature. •Beneficial surface hardened zones are formed at certain running-in conditions; the scientific background is presented here. •Ferritic-pearlitic steels strain hardens via grain size reduction and decreasing interlamellar distances in pearlite. •Austenitic steels show excellent surface hardening (120% hardness increase) by twinning and martensitic transformation. •Ferritic steels with hard phases harden in the ferrite phase as per Hall-Petch equation and degree of deformation.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Structural stability of mechanically alloyed amorphous (FeCoNi) 70 Ti 10 B 20 under high-temperature and high-pressure

Nanostructured (FeCoNi) 70 Ti 10 B 20 (at%) alloy was synthesized by mechanical alloying from elemental powder mixture of Fe, Co, Ni, Ti and B using ball milling. The effect of ball milling time on the evolution of structure and morphology was investigated by X-ray diffraction, scanning and transmission electron microscopy and differential thermal analysis. It was observed that the formation of solid solution of (FeCoNi) 70 Ti 10 B 20 started from the very onset of the milling process. Crystallite size and lattice strains seemed to be leveled off after 20 h of milling with no further major changes. The milling process for longer periods introduced severe plastic deformations causing formation of amorphous phase of (FeCoNi) 70 Ti 10 B 20 . The amorphous alloy composition was confirmed by energy dispersive X-ray spectroscopy analysis that showed an excellent homogeneity of the alloying elements. The phase stability of the mechanically alloyed amorphous sample was further verified by employing high-temperature and high-pressure studies. The alloy samples heat-treated at 700 °C revealed crystallization of the amorphous phase. However, synchrotron-based high-pressure ambient temperature X-ray diffraction studies confirmed that the amorphous phase of the alloy remained stable up to the pressure of 30 GPa. Here, the 50 h milled sample after being annealed at 350 °C showed improvement in the soft magnetic properties of the alloy, which was due to the probable elimination of the residual stress in the amorphous phase of the alloy powders.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Grain orientations and grain boundaries in tungsten nonotendril fuzz grown under divertor-like conditions

We grew nanotendril “fuzz” on tungsten via plasma exposure and performed transmission Kikuchi diffraction (tKD) in scanning electron microscopy of isolated nanotendrils. 900 °C, 10 23 He/m 2 sec, 4 × 10 26 He/m 2 exposure of tungsten produced a deep and fully developed nanotendril mat. tKD of isolated nanotendrils indicated that there was no preferred crystallographic direction oriented along the long axes of the tendrils, and the grain boundary character showed slightly preferential orientations. In conclusion, tendril growth is sufficiently non-equilibrium to prevent any preference of growth direction to manifest measurably, and that new high-angle boundaries (with new grains and grain-growth axes) nucleate randomly along the tendrils during growth.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2016

Characterization of reclaimed GaAs substrates and investigation of reuse for thin film InGaAlP LED epitaxial growth

This study reports a method to reuse GaAs substrates with a batch process for thin film light emitting diode (TF-LED) production. The method is based on an epitaxial lift-off technique. With the developed reclaim process, it is possible to get an epi-ready GaAs surface without additional time-consuming and expensive grinding/polishing processes. The reclaim and regrowth process was investigated with a one layer epitaxial test structure. The GaAs surface was characterized by an atomic force microscope directly after the reclaim process. The crystal structure of the regrown In{sub 0.5}(Ga{sub 0.45}Al{sub 0.55}){sub 0.5}P (Q{sub 55}) layer was investigated by high resolution x-ray diffraction and scanning transmission electron microscopy. In addition, a complete TF-LED grown on reclaimed GaAs substrates was electro-optically characterized on wafer level. The crystal structure of the epitaxial layers and the performance of the TF-LED grown on reclaimed substrates are not influenced by the developed reclaim process. This process would result in reducing costs for LEDs and reducing much arsenic waste for the benefit of a green semiconductor production.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2023

Analysis of neptunium oxides produced through modified direct denitration

Production of neptunium-237 ( 237 Np) target materials for plutonium-238 ( 238 Pu) radioisotope thermoelectric generators (RTGs) for deep space exploration requires advanced chemistry and engineering development. Currently, the domestic Pu-238 Supply Program at Oak Ridge National Laboratory produces neptunium dioxide (NpO 2 ) for target material using a modified direct denitration (MDD) flowsheet. Although the chemistry, reaction mechanisms, and product characteristics of MDD are well understood for uranium, corresponding studies of the neptunium system are still needed to continue optimization of target material properties, production equipment design, and production flowsheets. Here, the objective of this work is to characterize crystalline phases, morphology, surface texture, and particle size of NpO 2 produced via MDD reactions. Solid-phase characterization techniques, including powder X-ray diffraction (pXRD) and scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS), were employed to achieve this objective. Subsequent data processing using the Morphological Analysis for Material Attribution (MAMA) software was performed to analyze particle morphology and size. Broadly, the powders were found to contain a mixture of NpO 2 and Np 2 O 5 after denitration with a variety of morphologies. After high-firing, the product was found to be NpO 2 with a typical polycrystalline oxide morphology and a grain size ranging from 0.72 to 0.94 µm. These analyses provide knowledge on the reaction pathway for a non-traditional NpO 2 synthesis method and offer additional unique insight into production-scale environments for transuranic materials.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2017

Analysis of an MCU HEPA filter

A series of direct analyses on three portions (inlet, center, and outlet) of the High Efficiency Particulate Air (HEPA) filter material from the Modular Caustic-Side Solvent Extraction Unit (MCU) have been performed; this includes x-ray methods such as X-Ray Diffraction (XRD), Contained Scanning Electron Microscopy (CSEM) and X-Ray Fluorescence (XRF), as well as Fourier Transform InfraRed spectroscopy (FTIR). Additionally, two leaching studies (one with water, one with dichloromethane) have been performed on three portions (inlet, center, and outlet) of the HEPA filter material, with the leachates being analyzed by Inductively-coupled plasma emission spectroscopy (ICPES), Semi-Volatile Organic Analysis (SVOA) and gammascan. From the results of the analyses, SRNL feels that cesium-depleted solvent is being introduced into the HEPA filter. The most likely avenue for this is mechanical aerosolization of solvent, where the aerosol is then carried along an airstream into the HEPA filter. Once introduced into the HEPA filter media, the solvent wicks throughout the material, and migrates towards the outlet end. Once on the outlet end, continual drying could cause particulate flakes to exit the filter and travel farther down the airstream path.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2016

Studies on magnetic properties of chemically synthesized crystalline calcium ferrite nanoparticles

Spinel-type ferrites have taken a very important role for modern electronic industry. Most of these ferrites exhibit low-loss dielectric properties, high resistivity, low eddy current and also high temperature ferromagnetism. Calcium ferrite is one such important metal oxide which is environmentally safe, chemically stable, low cost and greatly abundant. This outstanding material of calcium ferrite is synthesized by a simple chemical precipitation method using NaOH as the precipitating agent. Ferric chloride anhydrous (FeCl{sub 3}) and Calcium chloride dihydrate (CaCl{sub 2}.2H{sub 2}O) were used as iron and calcium sources respectively. The samples were heated at 200°C for 8h to obtain homogeneous powder of Calcium ferrite. The powders were characterized by using X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), Transmission electrical microscopy (TEM), and Fourier transform infrared spectroscopic (FTIR) measurements. The polycrystalline nature of the sample was confirmed by X-ray diffraction study. The magnetic properties of the sample were investigated by vibrating sample magnetometer (VSM) measurements. Magnetization curve of the prepared sample depicts that as synthesized calcium ferrite nanoparticles have saturation magnetic moment of 1.74 emu/g and the coercivity of 35.08 Oe with superparamagnetic behavior. The synthesized calcium ferrite nanoparticles with such magnetic properties will be a candidate material for different applications in electronics and exploring its functionality in the field of recently developing semiconductor device physics and spintronics.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Ti-Nb thin films deposited by magnetron sputtering on stainless steel

Thin films of Ti-Nb alloys were deposited on AISI 316L stainless steel substrate by magnetron sputtering, and the structure, composition, morphology, and microstructure of the films were analyzed by means of x-ray diffraction (XRD), (scanning) transmission electron microscopy (TEM) coupled with energy-dispersive x-ray spectroscopy, atomic force microscopy (AFM), and x-ray photoelectron spectroscopy (XPS). Thin films of four compositions were produced: Ti{sub 85}Nb{sub 15} (Ti-26 wt. % Nb), Ti{sub 80}Nb{sub 20} (Ti-33 wt. % Nb), Ti{sub 70}Nb{sub 30} (Ti-45 wt. % Nb), and Ti{sub 60}Nb{sub 40} (Ti-56 wt. % Nb). Structural characterization by XRD indicated that only the β phase was present in the thin films and that the increase in the Nb content modified the alloy film texture. These changes in the film texture, also detected by TEM analysis, were attributed to different growth modes related to the Nb content in the alloy films. The mean grain sizes measured by AFM increased with the Nb amount (from 197 to 222 nm). XPS analysis showed a predominance of oxidized Ti and Nb on the film surfaces and an enrichment of Ti.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Understanding (La,Sr)(Co,Fe)O$_{3-δ}$ Phase Instability within SOECs Using a Combined Experimental and Atomistic Modeling Approach

Understanding the onset of degradation in the air electrode within solid oxide electrolysis cells (SOECs), and the subsequent impact on cell performance, is a critical step in mitigating the performance losses and stability issues of SOECs. In an effort to identify early onset degradation phenomena, SOECs were characterized as fabricated and after testing potentiostatically at 1.3 V for 1000 h at 750 °C. SOEC air electrodes composed of a 1:1 composite of La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3–δ (6428-LSCF) and Gd 0.1 Ce 0.9 O 1.95 (GDC) were studied using synchrotron X-ray diffraction (XRD), scanning transmission electron microscopy coupled with energy dispersive X-ray spectroscopy (STEM-EDS), and X-ray absorption near-edge spectroscopy (XANES) to evaluate the changes in the air electrode structurally and chemically. These techniques show the migration of Sr species from the air electrode through pores in the GDC barrier layer, progressing to the electrolyte boundary, where it accumulates and reacts with (Zr 0.84 Y 0.16 )O 2–δ (YSZ) to form SrZrO 3 . Microscopy results are paired with atomistic simulations to better understand the relationship between the thermodynamic instability of 6428-LSCF and cell fabrication/testing conditions. First-principles calculations reveal that LSCF-6428 is not stable during cell manufacturing and testing conditions, which supports the experimental identification of secondary phases in both as-fabricated and tested cells. Together, these results demonstrate that the challenging environments encountered by SOECs during cell manufacturing and operation lead to instabilities of the target 6428-LSCF anode material and underscore the need for more durable, high-performing SOEC components.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗