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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 235 records · Page 13
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Testing and Modeling of Functionally Graded Aluminum-Doped Zinc Oxide Using Spark Plasma Sintering and Discrete Powder Layers of Varying Composition

Functionally graded material (FGM) ZnO is made via spark plasma sintering/field-assisted sintering technique (SPS/FAST) by varying the Al dopant content along the z-axis or pressing direction. A wide range of Al content (0–5 wt%) is used by adding Al powder to nanosized ZnO powder. Thermoelectric (TE) measurements are done on the FGM and individual layers made separately. X-ray diffraction (XRD) shows two phases, ZnO and spinel phase (ZnAl 2 O 4 ). High-resolution Raman spectroscopy reveals doped ZnO and spinel phase (ZnAl 2 O 4 ) spatially and shows segregation in the layer with highest Al content. Electron backscatter diffraction (EBSD) reveals noticeable grain growth with decreasing Al content, and there is a common, random preferred orientation in all layers. The tested properties are used to simulate efficiency curves for a discretely graded, five-layer FGM as well as a homogenous material, where both graded structures provide an opportunity to widen the current density ranges and therefore the temperature range of useful energy conversion.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Transport and optical properties of the chiral semiconductor Ag 3 AuSe 2

Previous band structure calculations predicted Ag 3 AuSe 2 to be a semiconductor with a band gap of approximately 1 eV. Here, we report single crystal growth of Ag 3 AuSe 2 and its transport and optical properties. Single crystals of Ag 3 AuSe 2 were synthesized by slow-cooling from the melt, and grain sizes were confirmed to be greater than 2 mm using electron backscatter diffraction. Optical and transport measurements reveal that Ag 3 AuSe 2 is a highly resistive semiconductor with a band gap and activation energy around 0.3 eV. Our first-principles calculations show that the experimentally determined band gap lies between the predicted band gaps from GGA and hybrid functionals. We predict band inversion to be possible by applying tensile strain. The sensitivity of the gap to Ag/Au ordering, chemical substitution, and heat treatment merit further investigation.

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

Assessing Manufacturability of the Oxide Dispersion Strengthened (ODS) 14YWT Alloy Fuel Cladding Tube Using SolidStir™ Technology

The 14YWT (Fe–14Cr–3W–0.4Ti–0.3Y2O3 (wt.%)) alloy is a potential candidatematerial for fabricating fuel cladding tubes and other structural components to be used in next-generation advanced nuclear reactors. Due to inherent limitations of current processing routes, this research explored a new variant of friction stir processing, commercially referred to as SolidStir™ Extrusion (patent pending) technology from Enabled Engineering to consolidate and extrude 14YWT powder into a fuel cladding tube. Several single-layer and multiple-layer consolidation experiments were carried out in an Inconel 625 die to determine the suitable processing parameters for SolidStir™ extrusion of the 14YWT alloy cladding tube. With these processing parameters, a 16–18 mm long tube of the 14YWT alloy with no visible defects was successfully extruded using this novel technology. Microstructural characterization results obtained using optical microscopy, scanning electron microscopy, energy dispersive spectroscopy, electron backscatter diffraction, and transmission electron microscopy will be presented.

Advanced Materials and Manufacturing Technology↗
DOE OSTI2026

Process-driven roadmap for depositing super duplex stainless steel via wire Arc additive manufacturing

Here, this study systematically investigates the effects of shielding gas, bead spacing, weld mode, and travel speed on the phase balance, porosity, and hardness of wire arc additively manufactured (WAAM) super duplex stainless steel (ER2594). Robotic WAAM was employed to fabricate multilayer walls under systematically varied process conditions, followed by phase transformation simulations, X-ray computed tomography (XCT), electron backscatter diffraction (EBSD), and microhardness evaluation. Thermodynamic simulations predicted rapid cooling of AM process can suppress the potential formation of deleterious precipitates which was later validated via cross-sectional microstructure analyses of printed samples. XCT revealed porosity levels below 0.2% for all deposits, with reduced travel speed significantly lowering defect volume. Microstructural analyses revealed the evolution of various austenite precipitates, including grain boundary austenite (GBA), Widmanstätten austenite (WA), and intergranular austenite (IGA), sequentially upon cooling of the ferrite phase. Among all process parameters, weld transfer mode exhibited the strongest influence on phase balance; pulsed mode promoted higher ferrite retention (~ 36%) compared to RapidX mode. No consistent relationship between stabilized phase fraction and captured microhardness was observed. This work provides critical insights for optimizing WAAM parameters to control phase balance and mechanical performance, which is essential for producing high-integrity super duplex stainless-steel components for nuclear and marine applications.

Grain orientation↗
DOE OSTI2022

Spectroscopic identification of 2,3-dimethylbut-2-ene transients in 2,3-dimethylbut-2-ane flames

Combustion reactions provide the principal energy source of the world yet they are creating a burden through pollution. A detailed understanding of the complicated chemistry of flames is essential for optimizing energy output while minimizing detrimental side effects. Here, we present a measurement technique based on time domain, resonance-enhanced multiphoton ionization via Rydberg states followed by laser-induced plasma backscattering of microwaves and demonstrate this non-intrusive, in-situ technique by selectively identifying 2,3-dimethylbut-2-ene in a complex 2,3-dimethylbut-2-ane flame environment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Coastal-Fog Microphysics Using In-Situ Observations and GOES-R Retrievals

Here, the objective of this work is to evaluate GOES-R based fog conditions occurred during the C-FOG (Toward Improving Coastal Fog Prediction) field campaign. C-FOG is designed to advance understanding of fog formation, development, and dissipation over coastal environments to improve its predictability. The project took place along coastlines and open water environments of Eastern Canada (Nova Scotia, NS and the Island of Newfoundland, NL) during August-October of 2018 where environmental conditions play an important role for late season’s fog formation. During the C-FOG field campaign, instruments were located at the Ferryland Supersite, NL, with 2 main sites, and five satellite sites, as well as on the Research Vessel (R/V) Hugh R. Sharp. Key measurement instruments included a Gondola carrying a CDP (cloud droplet probe) and a BCP (backscatter cloud probe) was used for measuring droplet spectra from 1-75 µm on the R/V. A LPM (laser precipitation monitor) with 100 µm-1 cm size range and an OPC (optical particle counter) with 0.3-17 µm at 16 spectral channels provided information for fog and drizzle discrimination. Remote sensing platforms (e.g. profiling microwave radiometer, PMWR), Ceilometer, Lidar), meteorological towers, tethered balloons, and GOES-R products (e.g. fog coverage and droplet size and liquid water path) were used to evaluate fog over horizontal and vertical dimensions. Results suggest that effective radius, phase, liquid water path, and liquid water content values obtained from GOES-R and PMWR were comparable to ground based in-situ observations. It is concluded that integration of observations and nowcasting products may help improve short term local fog predictions.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2021

Analysis of Coastal Fog from a Ship During the C-FOG Campaign

This work presents ship-based measurements of fog off St John’s Newfoundland on 13 September 2018 during the Coastal Fog (C-FOG) field campaign. The measurements included cloud-particle spectra, cloud-base height and aerosol backscatter, radiation, turbulence, visibility, and sea surface temperature. Radiosonde soundings were made at intervals less than 2 hours. Fog occurred in two episodes under the center of eastward-moving synoptic low-pressure system. The boundary layer structure during the first fog episode consisted of 3 layers, separated by 2 saturated air temperature inversions and capped by a subsidence inversion. The lowest layer was fog and the upper layers were cloud. The second fog episode consisted of one well-mixed fog layer capped by a subsidence inversion. Low wind speeds and stable stratification maintained low surface-layer turbulence during fog. Droplet size distributions had typical bimodal distributions. The visibility correlated with the droplet number concentration and liquid water content. The air temperature was higher than the sea surface temperature for the first 30 minutes of the first fog episode but was colder than the sea for the remainder of all fog. The sensible heat flux was upward, from sea to air, for the first 62 % of the first fog episode and then reversed to downward, from air to sea, for the remainder of the first fog episode and the second fog episode. Here, the counter-gradient heat fluxes observed (i.e., opposite to what is expected from the instantaneous air-sea temperature difference) appear to be related to turbulence, entrainment and stratification in the fog layer that overwhelmed the influence of air-sea temperature difference. While the synoptic-scale dynamics preconditioned the area for fog formation, the final step of fog appearance in this case was nuanced by stratification-turbulence interactions, local advective processes and microphysical environment.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Boundary characterization using 3D mapping of geometrically necessary dislocations in AM Ta microstructure

Additive manufacturing (AM) of high strength metallic materials produces microstructures and defects that deviate substantially from those created through conventional manufacturing methods. It has recently been demonstrated that with application of extreme energy densities, a high-temperature refractory metal, tantalum (Ta), can be printed to a fully dense state with exceptionally low porosity. Here we employ a combination of three-dimensional electron backscattered diffraction (EBSD) TriBeam technology and crystallographic geometrically necessary dislocation (GND) theory to characterize the microstructure and defect boundaries of this unusual AM product. Two-dimensional (2D) EBSD and these three-dimensional (3D) measurements indicate that the microstructure of AM Ta is highly oriented <111> along the build direction, yet at the same time contains large crystallographic orientation gradients that span mm’s across the build. Crystallographic GND density analysis of the 3D microstructure reveals that highly misoriented subboundaries exist within this strongly textured microstructure that have large dislocation densities of 1×10 16 m –2 , just as large as those comprising the high-angle grain boundaries (HAGBs) in the same material. The 3D crystallographic GND density mapping reveals these subboundaries are part of a complex, finely spaced network that extends throughout the entire microstructure. Here, the orientation of these boundaries can be related to the scan strategy used during printing. TEM measurements corroborate an extremely high dislocation density at the microscale and indicate a cell-like dislocation network structure existing in the AM Ta at the sub-μm scale.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Using defects as a ‘fossil record’ to help interpret complex processes during additive manufacturing: as applied to raster-scanned electron beam powder bed additively manufactured Ti–6Al–4V

Abstract Defects in parts produced by additive manufacturing, instead of simply being perceived as deleterious, can act as important sources of information associated with the complex physical processes that occur during materials deposition and subsequent thermal cycles. Indeed, they act as materials-state ‘fossil’ records of the dynamic AM process. The approach of using defects as epoch-like records of prior history has been developed while studying additively manufactured Ti–6Al–4V and has given new insights into processes that may otherwise remain either obscured or unquantified. Analogous to ‘epochs,’ the evolution of these defects often is characterized by physics that span across a temporal length scale. To demonstrate this approach, a broad range of analyses including optical and electron microscopy, X-ray computed tomography, energy-dispersive spectroscopy, and electron backscatter diffraction have been used to characterize a raster-scanned electron beam Ti–6Al–4V sample. These analysis techniques provide key characteristics of defects such as their morphology, location within the part, complex compositional fields interacting with the defects, and structures on the free surfaces of defects. Observed defects have been classified as banding, spherical porosity, and lack of fusion. Banding is directly related to preferential evaporation of Al, which has an influence on mechanical properties. Lack-of-fusion defects can be used to understand columnar grain growth, fluid flow of melt pools, humping, and spattering events. Graphical abstract

36 MATERIALS SCIENCE↗
DOE OSTI2023

Differences in Oxidation Behavior of Conventionally Cast and Additively Manufactured Co-Base Alloy MAR-M-509

High-temperature oxidation behavior of conventionally cast and additively manufactured (AM) Co-base alloy MAR-M-509 was compared in the present study. The specimens were exposed in air at 1000 °C and characterized by means of scanning electron microscopy equipped with energy/wavelength dispersive x-ray spectroscopy (EDX/WDX) and electron backscatter diffraction as well as transmission electron microscopy. Substantial differences in the oxidation processes of two alloy versions were observed. Faster oxidation of the cast alloy was mainly induced by (1) oxidation of coarse primary carbides, (2) internal oxidation and nitridation processes and (3) incorporation of other alloy constituents (e.g., Co, Ni, W) into the Cr-oxide scale. AM specimens, in contrast, formed a more homogeneous, thinner and better adherent external oxide scale. The results are discussed in terms of differences in the chemical composition and alloy microstructure, including the grain size distribution in the material and the morphology of the strengthening precipitate phases.

36 MATERIALS SCIENCE↗
DOE OSTI2021

In-Situ SEM High Strain Rate Testing of Large Diameter Micropillars Followed by TEM and EBSD Postmortem Analysis

Background Dislocation dynamic simulations are intended as a tool to understand and predict the mechanical behavior of metallic materials, but its prediction has never been directly verified by experiments due to differences in specimen strain rate and size. Objective In this work, a comprehensive experimental framework is proposed to attempt direct comparison between experiments and discrete dislocation dynamics (DDD) modelling. Methods By integrating high-throughput sample fabrication and a customized testing apparatus, the sample size and strain rate typically employed in DDD simulations are explored experimentally. Constitutive properties such as stress-strain response are measured, and microstructural information is obtained from transmission electron microscopy (TEM) imaging, electron backscatter diffraction (EBSD), and TEM-based orientation mapping. Results Magnesium and copper were selected, as case studies, to demonstrate the newly developed experimental procedure. Measured stress-strain responses for Mg are consistent with those obtained with a miniaturized Hopkison bar experiments. Furthermore, by exploiting the validated workflow, the effect of strain rate on micropillar heterogeneous deformation and associated dislocation plasticity were revealed. Conclusion The work establishes a methodology for the systematic study of not only metals but also other materials and structures at the microscale and high strain rates.

42 ENGINEERING↗
DOE OSTI2021

Interrogating the Effects of Hydrogen on the Behavior of Planar Deformation Bands in Austenitic Stainless Steel

The effects of internal hydrogen on the deformation microstructures of 304L austenitic stainless steel have been characterized using electron backscattered diffraction (EBSD), transmission Kikuchi diffraction (TKD), high-resolution scanning transmission electron microscopy (HRSTEM), and nanoprobe diffraction. Samples, both thermally precharged with hydrogen and without thermal precharging, were subjected to tensile deformation of 5 and 20 pct true strain followed by multiple microscopic interrogations. Internal hydrogen produced widespread stacking faults within the as-forged initially unstrained material. While planar deformation bands developed with tensile strain in both the hydrogen-precharged and non-precharged material, the character of these bands changed with the presence of internal hydrogen. As shown by nanobeam diffraction and HRSTEM observations, in the absence of internal hydrogen, the bands were predominantly composed of twins, whereas for samples deformed in the presence of internal hydrogen, ε -martensite became more pronounced and the density of deformation bands increased. For the 20 pct strain condition, α '-martensite was observed at the intersection of ε -martensite bands in hydrogen-precharged samples, whereas in non-precharged samples α '-martensite was only observed along grain boundaries. We hypothesize that the increased prevalence of α '-martensite is a secondary effect of increased ε -martensite and deformation band density due to internal hydrogen and is not a signature of internal hydrogen itself.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Enhancement of Nanostructured Ferritic Alloy 14YWT Properties via Heat Treatment for Post-Consolidation Processing

The nanostructured ferritic alloy 14YWT is a promising candidate for in-core use in generation IV nuclear reactors, due to a dense dispersion of insoluble, ultrafine-scale Y-Ti-O nano-oxides, which provide a high degree of irradiation tolerance and thermal stability. This work investigates the effects of heat treatment on the workability of 14YWT, along with the effect of processing history on abnormal grain structures and radial microstructural uniformity. In this study, a 14YWT rod consolidated at 850 °C was heat treated in argon at 1100 °C, 1150 °C, 1200 °C, or 1250 °C for 1 or 8 hours and changes in mechanical properties and microstructure were examined using microhardness and electron backscattered diffraction (EBSD). Two distinct types of large abnormal grains were observed, each with unique processing origins, including one with high and the other with low strain energy. Consolidation via direct extrusion resulted in radial microstructural gradients, where the center of the rod was softer with larger grain sizes and lower strain energies. These gradients persisted and intensified throughout heat treatment. Based upon this work, the recommended heat treatment for increased workability with minimal microstructural change is 1150 °C for 1 hours.

36 MATERIALS SCIENCE↗
DOE OSTI2021

The Effect of Homogenization Heat Treatment on the Texture Evolution in U-10Mo Alloy

Uranium alloyed with 10 wt% Mo (U-10Mo) undergoes discontinuous precipitation (DP) when subjected to sub-eutectoid heat-treatment. It is hypothesized that the crystallographic texture of the U-10Mo can be modified to minimize the degree of DP, however the evolution of texture throughout the manufacturing process is not well understood. Crystallographic textures of two U-10Mo samples homogenized at 900°C and 1000°C were studied after uniaxial rolling and annealing. A total of 6 samples were analyzed upon rolling using a combination of hot and cold rolling conditions to strains of 83%, 90% and 97% and subsequently annealed at 700°C for one hour. Microstructures and textures were analyzed via electron backscatter diffraction (EBSD) for each homogenization, strain and post-annealed states. Results show that the U-10Mo exhibits typical rolling textures seen in body-centered cubic materials with increasing intensities of both a- and ?-fibers with increasing strain. After recrystallization, the texture appeared to be effectively randomized in all samples. Homogenization temperature showed no effect on the rolling and recrystallization behavior. Potential factors leading to the randomization of texture are discussed along with the implications of textures on the minimization of DP.

nuclear fuel, texture, rolling↗
DOE OSTI2021

Microstructural Analysis of Cadmium Whiskers on Long-Term-Used Hardware

A survey of cadmium plated field return hardware showed ubiquitous cadmium whisker growth. The most worn and debris-covered hardware showed the densest whisker growth. Whiskers were often found growing in agglomerates of nodules and whiskers. The hardware was rinsed with alcohol to transfer whiskers and debris from the hardware to a flat stub. Fifty whiskers were studied individually by scanning electron microscopy (SEM), including energy dispersive spectroscopy (EDS) and electron backscatter diffraction (EBSD). Most of the whiskers were single crystal, though three were found to contain grain boundaries at kinks. The whiskers ranged from 5 to 600 μm in length and 80 pct showed a $<\bar{1} 2 \bar{1} 0>$ type growth direction. This growth direction facilitates the development of low energy side faces of the whisker, (0001) and {1010}.

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 OSTI2023

An Integrated Simulation of Multiple-Pass U-10Mo Alloy Hot Rolling and Static Recrystallization

To achieve a desired microstructure and minimize the thickness variation in rolled foils, researchers must understand the effects of foil fabrication process variables on microstructure evolution. We developed an integrated simulation of deformation and recrystallization that employs the finite element method (FEM) and the kinetic Monte Carlo (KMC) Potts model, respectively, to investigate microstructure evolution during multiple-pass hot rolling and heat treatment in polycrystalline U-10Mo fuel. Scanning electron microscopy and electron backscatter diffraction images of microstructures were directly used as input in FEM calculation of deformation, and the calculated strains were used to determine the driving force of nucleation and growth of recrystallized grains in the Potts model. Grain structures predicted by the Potts model were used to update the grain structure and material properties for FEM. Simulation alternated between FEM and the Potts model to simulate grain structure evolution during multiple rolling and heat treatments. The initial model parameters were determined by benchmarking the recrystallization kinetics against experimental data. Then, the model was applied to predict the grain structure evolution. Results showed that our model can capture the coupling between deformation and recrystallization and can quantitatively reproduce the observed U-10Mo recrystallization and grain growth kinetics. The simulation results demonstrated that the developed model can predict U-10Mo grain structures as a function of initial microstructure and foil fabrication parameters.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Characterization and Rationalization of Microstructural Evolution in GRCop-84 Processed by Laser-Powder Bed Fusion (L-PBF)

In this study, prismatic geometries of GRCop-84 [Cu-8Cr-4Nb (at. pct)] were built with laser-powder bed fusion (L-PBF) process. The samples were sectioned parallel or perpendicular to the build direction and characterized in the as-built and after post-processing with a hot-isostatically pressing (HIP) treatment. The microstructure and phase evolutions were evaluated with optical microscopy, scanning electron microscopy (SEM), electron backscattered diffraction (EBSD), and high-temperature X-ray diffraction (HTXRD) up to 1223 K. The samples in the as-built conditions exhibited predominantly columnar epitaxial and misoriented Cu-FCC grains. The microstructure evolutions are discussed based on locations within the overall build geometry, the dynamics of small melt pool shape and sectioning effects. The above grain structure did not change significantly during post-process HIP treatment. The stability of this FCC grain structure is attributed to the formation of primary stable Cr 2 Nb (Laves phase) during L-PBF, even before the emergence of FCC grains from liquid. The stability of Cr 2 Nb in both as-built and HIPed samples were evaluated using high-temperature X-ray diffraction measurements and compared with that of gas-atomized powder. The significance of these results is discussed with reference to aerospace applications.

36 MATERIALS SCIENCE↗