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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 793 records · Page 44
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

High-strength bioresorbable Fe–Ag nanocomposite scaffolds: Processing and properties

High strength ductile iron-silver nanocomposite scaffolds were fabricated employing high energy attrition milling of micron-submicron powders, followed by cold sintering/high pressure consolidation. Particulate leaching method with soluble Na{sub 2}SO{sub 4} and K{sub 2}CO{sub 3} salts as porogens was used to create scaffolds with 50, 55, 60 and 73% volume fraction of pores. Part of specimens was annealed at 600, 800 and 900°C. Specimens were characterized employing X-ray diffraction, scanning electron microscopy (SEM) with electron probe microanalysis (EDS) and high resolution SEM. Mechanical properties were measured in compression and permeability was measured in permeameter based on Darcy’s law. Scaffolds with 50% and 55% porosity exhibited high compressive strength (18–22 MPa), compressive strength of 8–12 MPa was observed for scaffolds with 73% porosity. Treatments at 800 and 900°C result in increase of strength and ductility with some coarsening of microstructure. Best combination of compressive strength (15 MPa) and permeability (0.6{sup −6} cm{sup 2}) is close to the range of trabecular bone.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of as-cast microstructure heterogeneity on aging behavior of a high-pressure die-cast A380 alloy

Highlights: • The surface layer hardened much faster than the central region during age. • More quantity of finer precipitates was found in the surface layer during age. • The surface layer had a lower activation energy of precipitation. • Si promoted the precipitation via inducing dislocations in matrix. - Abstract: Microstructure and hardness evolution of a vacuum-assistant die-cast A380 alloy during heat treatment were investigated. Both surface layer and central region of the casting component were analyzed in die-cast state, solutionized state and artificial age state. During the artificial age, the surface layer hardened more significantly than the central region due to faster precipitation and more refined hardening phases in the surface layer. Detailed analysis on the macro-segregation, microstructure morphology and grain size revealed that the different aging behaviors exhibiting in the surface and the central region were mainly attributed to a combining effect of the enrichment of Si and Cu at the surface layer, the fully-divorced morphology of eutectic in die-cast microstructure, and the presence of the externally solidified crystals at the central region. The presence of the Si particles, which exhibited quite different thermal expansion properties, changed the density and the distribution of the dislocations in the α-Al matrix, and consequently changed the precipitation of the hardening phases.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Influence of Two Different Salt Mixture Combinations of Na{sub 2}SO{sub 4}-NaCl-NaVO{sub 3} on Hot Corrosion Behavior of Ni-Base Superalloy Nimonic263 at 800 °C

Isothermal hot corrosion behavior of Nimonic263 alloy was studied under the influence of two different salt mixtures of 87.5 wt.% Na{sub 2}SO{sub 4} + 5 wt.% NaCl + 7.5 wt.% NaVO{sub 3} (3SM) and 74 wt.% Na{sub 2}SO{sub 4} + 21.7 wt.% NaCl + 4.3 wt.% NaVO{sub 3} (3SM-A) and also without salt mixtures up to 500 h at 800 °C. Corrosion kinetics showed that 3SM-A is more aggressive than 3SM. Multiple oxides, spinels, sulfides, vanadate compounds, and volatile compounds were observed during various hot corrosion reactions. The volatile compounds NaClO{sub 3} and CrMoO{sub 3}, and SO{sub 3} gas are attributed to the weight loss under both 3SMs. The Na{sub 2}SO{sub 4} of 3SM prevailed till 400 h, but that of 3SM-A disappeared within 5 h, as established conclusively by Raman spectra analysis. The sulfides plus internal oxide zone increased with the increased exposure duration as evident from the extensive EPMA analysis. Based on the critical analysis of corrosion kinetics and detailed microstructural characterization, fluxing and sulfidation followed by oxidation are identified as plausible hot corrosion mechanisms under both 3SMs. Besides, chlorination and high-temperature oxidation mechanisms occur under 3SM-A condition.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Surface Layers of Zr-18%Nb Alloy Modified by Ultrasonic Impact Treatment: Microstructure, Hardness and Corrosion

Near-surface layers in Zr-18%Nb alloy were modified using ultrasonic impact treatment (UIT). The effects of the UIT processing time on a microstructural formation, omega/alpha precipitations, microhardness and corrosion are analyzed. XRD analysis, TEM and SEM observations and EDX characterization allow establishing the links between the microstructure, microhardness and corrosion behavior of the surface layers formed. At the strain extent up to e ≈ 0.3, structural formation occurs under influence of deformation induced heating, which facilitates omega precipitation in beta phase and mechanically induced oxygen transport and oxide formation. XRD analysis reveals moderate compressive residual stresses (− 160 MPa) and pronounced {110} texture after the UIT process. Generation of dislocations and hindering of their movement by nanoscale omega precipitates manifest themselves as the broadening of diffraction peaks occurred mainly owing to the lattice microstrains, and they provide marked strain hardening. The enhanced anticorrosion properties of Zr-18%Nb alloy in saline solution were concluded to be a result of the formation of a protective oxide film, {110} texture and compressive stresses.

36 MATERIALS SCIENCE↗
DOE OSTI2017

The influence of substrate moisture preparation on bond strength of concrete overlays and the microstructure of the OTZ

The influence of substrate moisture preparation on the direct shear bond strength of composite substrate-overlay specimens was evaluated. The substrate surface was exposed to four different moisture conditions prior to overlay application. A quantitative analysis of backscattered electron images of the microstructure of the overlay transition zone was carried out to quantify its properties along the interface and help analyse the results of the shear bond testing. The results show that pre-wetting the substrate surface prior to application of the overlay provides no added benefit towards increasing the bond strength and may in some cases reduce bond strength significantly. The microstructural investigations confirmed that pre-saturated substrates increase the w/c ratio and the porosity in the overlay transition zone (OTZ), which was found to have a thickness of about 100 μm. The OTZ in overlays cast on dry substrate surfaces had lower porosity and an increased amount of anhydrous cement.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Three-dimensional (3D) analysis of white etching bands (WEBs) in AISI M50 bearing steel using automated serial sectioning

Dark etching regions (DER) and white etching bands (WEB) form in the subsurface stressed regions of bearing raceways and rolling elements. Also, “butterfly” formations form around non-metallic inclusions and large carbides. The formation of WEBs, DERs and butterfly are dependent on operating conditions, material alloying elements and heat treatment. The DER, WEB and butterfly formations are well studied in two dimensions (2D). The objective of this study was to analyze WEB formation in three dimensions (3D) that will allow better understanding of material transformation after stress cycling. Three rolling contact fatigue (RCF) tested vacuum induction melted vacuum arc re-melted (VIM-VAR) AISI M50 samples (from a bench test, sub-scale test and commercial gas turbine engine) were analyzed using automated serial sectioning to map WEB networks and a butterfly formation in 3D. Automated serial sectioning and 2D optical microstructural data for 3D reconstructions and analysis was done using a fully automated serial sectioning system – Robo-Met.3D®. 3D analysis was performed using Image-Pro Premier 3D. The data set allowed 3D visualization and analysis of the evolution and propagation of WEB and butterfly in M50 bearing steel, including the positive microscopic identification of a ceramic inclusion that was the source of a WEB.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Polarized quasiperiodic structures in pulsar radio emission reflect temporal modulations of non-stationary plasma flow

Bright single pulses of many radio pulsars show rapid intensity fluctuations (called microstructure) when observed with time resolutions of tens of microseconds. Here, we report an analysis of Arecibo 59.5 μs resolution polarimetric observations of 11 P-band and 32 L-band pulsars with periods ranging from 150 ms to 3.7 s. These higher-frequency observations form the most reliable basis for detailed microstructure studies. Close inspection of individual pulses reveals that most pulses exhibit quasi-periodicities with a well-defined periodicity timescale (P{sub μ}). While we find some pulses with deeply modulating microstructure, most pulses show low-amplitude modulations on top of broad smooth subpulse features, thereby making it difficult to infer periodicities. We have developed a method for such low-amplitude fluctuations wherein a smooth subpulse envelope is subtracted from each de-noised subpulse; the fluctuating portion of each subpulse is then used to estimate P{sub μ} via autocorrelation analysis. We find that the microstructure timescale P{sub μ} is common across all Stokes parameters of polarized pulsar signals. Moreover, no clear signature of curvature radiation in vacuum in highly resolved microstructures was found. Our analysis further shows strong correlation between P{sub μ} and the pulsar period P. We discuss implications of this result in terms of a coherent radiation model wherein radio emission arises due to formation and acceleration of electron–positron pairs in an inner vacuum gap over magnetic polar cap, and a subpulse corresponds to a series of non-stationary sparking discharges. We argue that in this model, P{sub μ} reflects the temporal modulation of non-stationary plasma flow.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2014

3D characterization of trans- and inter-lamellar fatigue crack in (α + β) Ti alloy

This paper presents a three dimensional image processing strategy that has been developed to quantitatively analyze and correlate the path of a fatigue crack with the lamellar microstructure found in Ti-6246. The analysis is carried out on X-ray microtomography images acquired in situ during uniaxial fatigue testing. The crack, the primary β-grain boundaries and the α lamellae have been segmented separately and merged for the first time to allow a better characterization and understanding of their mutual interaction. This has particularly emphasized the role of translamellar crack growth at a very high propagation angle with regard to the lamellar orientation, supporting the central role of colonies favorably oriented for basal 〈a〉 slip to guide the crack in the fully lamellar microstructure of Ti alloy. - Highlights: • 3D tomography images reveal strong short fatigue crack interaction with α lamellae. • Proposed 3D image processing methodology makes their segmentation possible. • Crack-lamellae orientation maps show prevalence of translamellar cracking. • Angle study comforts the influence of basal/prismatic slip on crack path.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Improved microstructure of cement-based composites through the addition of rock wool particles

Rock wool is an inorganic fibrous substance produced by steam blasting and cooling molten glass. As with other industrial by-products, rock wool particles can be used as cementitious materials or ultra fine fillers in cement-based composites. This study investigated the microstructure of mortar specimens produced with cement-based composites that include various forms of rock wool particles. It conducted compressive strength testing, rapid chloride penetration tests, X-ray diffraction analysis, thermo-gravimetric analysis, and scanning electronic microscopy to evaluate the macro- and micro-properties of the cement-based composites. Test results indicate that inclusion of rock wool particles in composites improved compressive strength and reduced chloride ion penetration at the age of 91 days due to the reduction of calcium hydroxide content. Microscopic analysis confirms that the use of rock wool particles contributed to the formation of a denser, more compact microstructure within the hardened paste. In addition, X-ray diffraction analysis shows few changes in formation of pozzolanic reaction products and no new hydrations are formed with incorporating rock wool particles. - Highlights: • We report the microstructural characterization of cement-based composites. • Different mixes produced with various rock wool particles have been tested. • The influence of different mixes on macro and micro properties has been discussed. • The macro properties are included compressive strength and permeability. • XRD and SEM observations confirm the pozzolanic reaction in the resulting pastes.

36 MATERIALS SCIENCE↗
DOE OSTI2025

In-Situ Synchrotron X-Ray Diffraction of Ultrasonic Microstructural Refinement During Solidification in a Commercial Al–Si–Mg Alloy

This study reports the first use of in-situ synchrotron X-ray diffraction (SXRD) to study the effects of ultrasonic melt processing (USMP) on phase and grain size evolution during solidification in a commercial Al–Si–Mg casting alloy. USMP is a technique that, when applied to aluminum as it solidifies, can be used to refine the local microstructure of large-scale castings. Analysis of the in-situ SXRD data to estimate the average grain size of primary α-Al grains during USMP demonstrates that USMP slows the growth rate of α-Al grains and reduces grain size by 36 pct. Furthermore, there is also evidence that USMP causes the primary α-Al grains to move relative to the X-ray beam; such motion increases the probability of primary α-Al grains colliding and fragmenting. This movement becomes constrained at the onset of the Al–Si binary eutectic, suggesting that USMP ceases to effectively refine the microstructure once the Al–Si binary eutectic begins to form. Complementary laboratory-scale X-ray diffraction (XRD) data were used to correlate the lattice parameters of the α-Al and Si (D-A4) phases with temperature to estimate cooling rate during solidification. Thus, this study can guide the design of novel castings with spatially distributed fine-grained regions produced using local ultrasonic processing.

Aluminum Alloys↗
DOE OSTI2016

Failure mechanisms of single-crystal silicon electrodes in lithium-ion batteries

Long-term durability is a major obstacle limiting the widespread use of lithium-ion batteries in heavy-duty applications and others demanding extended lifetime. As one of the root causes of the degradation of battery performance, the electrode failure mechanisms are still unknown. In this paper, we reveal the fundamental fracture mechanisms of single-crystal silicon electrodes over extended lithiation/delithiation cycles, using electrochemical testing, microstructure characterization, fracture mechanics and finite element analysis. Anisotropic lithium invasion causes crack initiation perpendicular to the electrode surface, followed by growth through the electrode thickness. The low fracture energy of the lithiated/unlithiated silicon interface provides a weak microstructural path for crack deflection, accounting for the crack patterns and delamination observed after repeated cycling. On the basis of this physical understanding, we demonstrate how electrolyte additives can heal electrode cracks and provide strategies to enhance the fracture resistance in future lithium-ion batteries from surface chemical, electrochemical and material science perspectives.

25 ENERGY STORAGE↗
DOE OSTI2019

Two-Magnon Relaxation Processes in Nanocrystalline Thin Magnetic Films

Numerical analysis of the micromagnetic model was used to reveal the ‘resonance’ feature of relaxation processes in nanocrystalline thin magnetic films. This feature manifests itself in the form of sharp broadening of the ferromagnetic resonance (FMR) line at a certain frequency f{sub 1} depending on magnetic characteristics of the film, and is observed only in films the thickness of which exceeds some threshold value d{sub min}. Sharp broadening of the FMR line is accompanied by significant shift of the resonance field, whereas the shift value changes the sign at frequency ~ f{sub 1}. It was shown analytically that the nature of observed effects is associated with the two-magnon process of spin waves scattering on quasi-periodic magnetic microstructure – magnetization ‘ripple’. Obtained expressions for the threshold value of film thickness d{sub min} and frequency of maximum broadening of FMR line f{sub 1} agree well with the results of numerical computation of micromagnetic model.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Exascale granular microstructure reconstruction in 3D volumes of arbitrary geometries with generative learning

Reconstructing 3D granular microstructures within volumes of arbitrary geometries from limited 2D image data is crucial for predicting the material properties, as well as performances of structural components accounting for material microstructural effects. We present a novel generative learning framework that enables exascale reconstruction of granular microstructures within complex 3D geometric volumes. Building upon existing transfer learning techniques using pre-trained convolutional neural networks (CNN), we introduce several key innovations to overcome the difficulties inherent in arbitrary geometries. Our framework incorporates periodic boundary conditions using circular padding techniques, ensuring continuity and representativeness of the reconstructed microstructures. We also introduce a novel seamless transition reconstruction (STR) method that creates statistically equivalent transition zones to integrate multiple pre-existing 3D microstructure volumes. Based on STR, we propose a cost-effective strategy for reconstructing microstructures within complex geometric volumes, minimizing computational waste. Validation through numerical experiments using kinetic Monte Carlo simulations demonstrates accurate reproduction of grain statistics, including grain size distributions and morphology. A case study involving the reconstruction of a 4-blade propeller microstructure illustrates the method’s capability to efficiently handle complex geometries. In conclusion, the proposed framework significantly reduces computational demands while maintaining high reconstruction quality, paving the way for scalable microstructure reconstruction in materials design and analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Effect of calcite filler on carbonation behavior in a synthesized C‐S‐H binder

Widespread implementation of portland limestone cements (PLC) in industry has raised new questions about their carbonation resistance due to higher initial limestone content than ordinary portland cement. While carbonation of portland cement and each of its hydrate phases has been studied at a fundamental level, the integral role of how limestone fillers interact chemically or physically during carbonation necessitates further study. In this study, a C-S-H binder comprised of a highly reactive zeolite pozzolan and lime was used to evaluate the effect of varying calcite additions on carbonation behavior at a microstructural level. Fundamental insight into hydration kinetics and carbonation mechanisms of hydraulic binders was obtained via analysis of the C-S-H and calcite microstructure. X-ray microcomputed tomography (X-ray CT) was used to quantify microstructural changes, and the results showed a decrease in shrinkage for increased calcite dosages, with a ∼50% reduction observed for a 45% wt. calcite replacement level. Crystallographic and thermal analyses measured compositional changes in the binder and confirmed that shrinkage was related to the decalcification of C-S-H. Furthermore, the addition of calcite to the C-S-H binder effectively reduced the liquid-to-solid ratio, porosity, and amount of C-S-H present in these binders. Ultimately, these results help elucidate how the carbonation risks of PLC can be mitigated by proportioning the mixture water only to the reactive component of the binder.

C-S-H↗
DOE OSTI2025

Computational materials reliability assessment of hydrogen fueled gas turbine power generation engines

The use of blended fuel sources in land based gas turbine engines drives variations in the resulting operational profile (temperatures and pressures) which can impact engine reliability. Furthermore, variability in the manufacture of components affects the resulting microstructure which directly impacts material performance and reliability. Currently, data-driven models are typically used for maintaining and inspecting fleets of engines. Without explicitly capturing material and operational sources of variability conservatism must be used in developing component-level reliability models. Therefore, there exists an opportunity to use information from materials-scale physics models to better inform reliability modeling and reduce conservatism; the impact is more cost-efficient operation and maintenance of current and future fleets. Specifically, this work establishes a computational framework for evaluating the probabilistic high temperature creep performance of hot-section Ni-based superalloys where uncertainty comes from both microstructural and operational variability. A novel high-fidelity physics model which phenomenologically captures grain-boundary sensitive phenomena has been established. A probabilistic calibration procedure was used to calibrate the model and capture uncertainty in the parameterized model coefficients. A design of experiments methodology was established for identifying informative microstructural digital representations for suitable for forward model evaluation. Results show that training a machine-learning surrogate using this design criteria outperforms random selection of microstructural representations. Finally, two surrogate models were developed: (1) a deterministic surrogate model which predicts the local field response given microstructure, constitutive model parameters, and operating conditions (stress, temperature) and (2) a probabilistic model, where uncertainty comes from constitutive law uncertainty, built using denoising diffusion probabilistic models which samples responses given (1) microstructure and (2) operating conditions. These surrogate models enable partner Siemens Energy to rapidly perform UQ analysis specific to creep deformation across a range of microstructures and operating conditions. The impact is that these ML and physics codes can be used to establish more advanced reliability models for the inspection, servicing, and maintenance of land based gas turbine engines.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Electron scattering mechanisms in GZO films grown on a-sapphire substrates by plasma-enhanced molecular beam epitaxy

We report on the mechanisms governing electron transport using a comprehensive set of ZnO layers heavily doped with Ga (GZO) grown by plasma-enhanced molecular-beam epitaxy on a-plane sapphire substrates with varying oxygen-to-metal ratios and Ga fluxes. The analyses were conducted by temperature dependent Hall measurements which were supported by microstructural investigations as well. Highly degenerate GZO layers with n > 5 x 10{sup 20} cm{sup -3} grown under metal-rich conditions (reactive oxygen-to-metal ratio <1) show relatively larger grains ({approx}20-25 nm by x-ray diffraction) with low-angle boundaries parallel to the polar c-direction. For highly conductive GZO layers, ionized-impurity scattering with almost no compensation is the dominant mechanism limiting the mobility in the temperature range from 15 to 330 K and the grain-boundary scattering governed by quantum-mechanical tunnelling is negligible. However, due to the polar nature of ZnO having high crystalline quality, polar optical phonon scattering cannot be neglected for temperatures above 150 K, because it further reduces mobility although its effect is still substantially weaker than the ionized impurity scattering even at room temperature (RT). Analysis of transport measurements and sample microstructures by x-ray diffraction and transmission electron microscopy led to a correlation between the grain sizes in these layers and mobility even for samples with a carrier concentration in the upper 10{sup 20} cm{sup -3} range. In contrast, electron transport in GZO layers grown under oxygen-rich conditions (reactive oxygen-to-metal ratio >1), which have inclined grain boundaries and relatively smaller grain sizes of 10-20 nm by x-ray diffraction, is mainly limited by compensation caused by acceptor-type point-defect complexes, presumably (Ga{sub Zn}-V{sub Zn}), and scattering on grain boundaries. The GZO layers with n <10{sup 20} cm{sup -3} grown under metal-rich conditions with reduced Ga fluxes show a clear signature of grain-boundary scattering governed by the thermionic effect in the temperature-dependent mobility but with much higher RT mobility values compared to the samples grown under oxygen-rich conditions [34 vs. 7.5 cm{sup 2}/V{center_dot}s]. Properties of GZO layers grown under different conditions clearly indicate that to achieve highly conductive GZO, metal-rich conditions instead of oxygen-rich conditions have to be used.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Solid-state reaction mediated microstructural evolution in a spark plasma sintered in situ Ti–B 4 C composite

For this study, a novel porosity-free in situ Ti–B 4 C composite was fabricated via spark plasma sintering (SPS). Detailed analysis of the phase evolution, coupling results from XRM, XRD and SEM-EBSD-EDS, indicate that primarily TiB 2 precipitates formed due to the in-situ reactions between the boron-carbide and titanium powders. The precipitation of TiB 2 resulted in the formation of a graphitic C-rich thin layer circumscribing the partially reacted B 4 C particles. Further progression of the in-situ reaction leads to the out-diffusion of the excess carbon from the B 4 C particles, across the graphite and TiB 2 phases, forming TiC upon reacting with the titanium matrix. Therefore, the final microstructure primarily consisted of TiB 2 , TiC, and partially reacted B 4 C phases, with small amounts of TiB, α-Ti, and graphite. Furthermore, the microstructure in these SPS processed in situ composites appeared to be the product of a solid-state Ti–B 4 C diffusion couple, substantially different from their fusion-based additively manufactured counterparts. Nano-indentation tests revealed a remarkably high average hardness of ~25 GPa for this SPS-processed Ti–B 4 C composite and comparable (with literature) phase-specific hardness and modulus values for the constituent TiB 2 , TiC, and B 4 C phases.

36 MATERIALS SCIENCE↗