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At least 703 records · Page 39
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Constitutional under-potential plating (CUP) – New insights for predicting the morphological stability of deposited lithium anodes in lithium metal batteries

Lithium (Li) cycling in lithium metal batteries (LMBs) inevitably witnesses a non-planar Li/electrolyte interface (cellular/dendritic microstructure) affecting the performance, safety and reliability of LMBs. Herein, the “constitutional under-potential plating” (CUP) concept is presented for the first time to understand the evolution, formation and predict the morphological stability/instability of the Li/electrolyte interface. Here, the CUP condition, a measure of the driving force for interface perturbation, occurs when the true potential gradient at the interface is smaller than the equilibrium electrodeposition potential gradient at the Li/electrolyte interface resulting in the electrolyte ahead of the Li-electrolyte interface to be in an under-potential state. Detailed CUP criterion calculations conducted herein establishes the relationship of battery operating conditions (e.g. current density, potential gradient) with the electrolyte properties (e.g. Li-ion transference number and diffusion coefficient) predicting the morphological stability condition at the interface. In addition to the driving force for interface perturbation, the capillarity effect or the Gibbs Thomson effect, a measure of the resistance to perturbation of the perturbed interface is discussed for understanding the influence of interfacial energy/adhesion energy between the current collector and the deposited Li on the overall morphological stability of the Li/electrolyte interface, a critical criterion for the unwanted dendritic morphology.

25 ENERGY STORAGE↗
DOE OSTI2025

High resolution microstructural, chemical studies and localized burnup analysis in an irradiated U–10Zr metallic fuel

This study involves high resolution characterization of a sodium bonded solid uranium (U)-10 wt% zirconium (Zr) metallic fuel irradiated in Fast Flux Test Facility (FFTF). The fuel centerline temperature during irradiation was estimated to be around 675 °C with the peak burnup 13.1 atomic percent. Samples for transmission electron microscopy (TEM) and atom probe tomography (APT) were prepared from different regions/zones in the fuel cross section radially to elucidate the microstructural changes and chemical redistribution of solute elements as well as fission products during irradiation experiment. TEM results indicate the irradiation in fast flux testing leads to the formation of extensive Zr-rich precipitates with varying sizes in the U–Zr fuel matrix. APT analysis performed to investigate redistribution of Zr, U and fission products along the radial direction of fuel pin showed Zr-rich precipitates entrapping the fission products in higher concentration as compared to the α-U phases. Here, the local burnup ( 235 U depletion) is found to be consistent, calculated by quantification of 235 U, 236 U and 238 U isotopes from mass spectrum obtained from APT along the radial direction. Zr-rich precipitation and its implication on fuel constitutional redistribution are discussed based on SEM, TEM and APT results.

APT↗
DOE OSTI2021

Self-Assembled BaTiO 3 –Au x Ag 1– x Low-Loss Hybrid Plasmonic Metamaterials with an Ordered “Nano-Domino-like” Microstructure

Metallic plasmonic hybrid nanostructures have attracted enormous research interest due to the combined physical properties coming from different material components and the broad range of applications in nanophotonic and electronic devices. However, the high loss and narrow range of property tunability of the metallic hybrid materials have limited their practical applications. In this study, a metallic alloy-based self-assembled plasmonic hybrid nanostructure, i.e., a BaTiO 3 –Au x Ag 1– x (BTO) vertically aligned nanocomposite, has been integrated by a templated growth method for low-loss plasmonic systems. Comprehensive microstructural characterizations including high-resolution scanning transmission electron microscopy (HRSTEM), energy-dispersive X-ray spectroscopy (EDS), and three-dimensional (3D) electron tomography demonstrate the formation of an ordered “nano-domino-like” morphology with Au 0.4 Ag 0.6 nanopillars as cylindrical cores and BTO as square shells. By comparing with the BTO–Au hybrid thin film, the BTO–Au 0.4 Ag 0.6 alloyed film exhibits much broader plasmon resonance, hyperbolic dispersion, low-loss, and thermally robust features in the UV–vis–NIR wavelength region. This study provides a feasible platform for a complex alloyed plasmonic hybrid material design with low-loss and highly tunable optical properties toward all-optical integrated devices.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Diversifying Composition Leads to Hierarchical Composites with Design Flexibility and Structural Fidelity

Although significant progress has been made in the self-assembly of nanostructures, present successes heavily rely on precision in building block design, composition, and pair interactions. These requirements fundamentally limit our ability to synthesize macroscopic materials where the likelihood of impurity inclusion escalates and, more importantly, to access molecular-to-nanoscopic-to-microscopic-to-macroscopic hierarchies, since the types and compositions of building blocks vary at each stage. Inspired by biological blends and high-entropy alloys, we hypothesize that diversifying the blend’s composition can overcome these limitations. Increasing the number of components increases mixing entropy, leading to the dispersion of different components and, as a result, enhances interphase miscibility, weakens the dependence on specific pair interactions, and enables long-range cooperativity. This hypothesis is validated in complex blends containing small molecules, block copolymer-based supramolecules, and nanoparticles/colloidal particles. Hierarchically structured composites can be obtained with formulation flexibility in the filler selection and blend composition. It is worth noting that, by adding small molecules, we can solve the size constraint that plagues traditional block copolymer/nanoparticle blends. Detailed characterization and simulation further confirm that each component is distributed to locally mediate unfavorable interactions, cooperatively mitigate composition fluctuations, and retain structural fidelity. Furthermore, the blends have sufficient mobility to access tunable microstructures without compromising the order of the nanostructure. Besides establishing a kinetically viable pathway to release current constraints in the composite design and to navigate uncertainties during structure formation over multiple length scales, the present study demonstrates that entropy-driven behaviors can be realized in systems beyond high-entropy alloys despite inherent differences between metal alloys and organic/inorganic hybrids.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2003

Alumina Volatility in Water Vapor at Elevated Temperatures

The volatility of alumina in high temperature water vapor was determined by a weight loss technique. Sapphire coupons were exposed at temperatures between 1250 and 1500 C, water partial pressures between 0.15 and 0.68 atm in oxygen, total pressure of 1 atm, and flowing gas velocities of 4.4 cm/s. The pressure dependence of sapphire volatility was consistent with AI(OH)3(g) formation. The enthalpy of reaction to form Al(OH)3(g) from sapphire and water vapor was determined to be 210 +/- 20 kJ/mol, comparing favorably to other studies. Microstructural examination of tested sapphire coupons revealed surface etching features consistent with a volatilization process.

Opila, Elizabeth J.↗
NASA NTRS2009

Coordinated Stem and NanoSIMS Analysis of Enstatite Whiskers in Interplanetary Dust Particles

Enstatite whiskers (less than 10 micrometer length, less than 200 nanometer width) occur in chondritic-porous interplanetary dust particles (CP IDPs), an Antarctic micrometeorite and a comet 81P/Wild-2 sample. The whiskers are typically elongated along the [100] axis and contain axial screw dislocations, while those in terrestrial rocks and meteorites are elongated along [001]. The unique crystal morphologies and microstructures are consistent with the enstatite whiskers condensing above approximately 1300 K in a low-pressure nebular or circumstellar gas. To constrain the site of enstatite whisker formation, we carried out coordinated mineralogical, chemical and oxygen isotope measurements on enstatite whiskers in a CP IDP.

Nakamura-Messenger, K.↗
DOE OSTI2021

Unravelling chloride transport/microstructure relationships for blended-cement pastes with the mini-migration method

A chloride mini-migration method is proposed to estimate effective diffusion coefficients at the scale of the cement paste and to investigate mechanisms with complementary microstructure analyses on the same material. Blended-cement pastes with a wide range of properties were investigated in this study: systems at w/b = 0.3–0.5 including Portland cement, white Portland cement, slag-Portland cement, fly ash, glass powder, and/or limestone and calcined clay. Comparisons showed the relative and combined importance of three main parameters on the effective diffusion coefficient: the porosity, the pore connectivity parameter and the conductivity of the pore solution (low values of the latter two are generally key aspects of the high resistance of blended-cement systems against chloride ingress). Notably, a general correlation for all the investigated systems was established between the effective diffusion coefficient and the bulk conductivity (whereas no simple correlation was observed between the effective diffusion coefficient and the formation factor or the pore connectivity parameter).

36 MATERIALS SCIENCE↗
NASA NTRS2016

Macrosegregation and Grain Formation Caused by Convection Associated with Directional Solidification Through Cross-Section Increase

Cylindrical Al-7 wt% Silicon, Al-19 wt% Copper and Lead-6 wt% Antimony alloy samples were directionally solidified (DS) with liquid above, solid below, and gravity pointing down, in graphite crucibles having an abrupt cross-sectional increase. These alloys have similar solidification shrinkage but are expected to have different degrees of thermosolutal convection during solidification. Microstructures in the DS samples in the vicinity of the section change have been studied in order to examine the effect of convection associated with the combined influence of thermosolutal effects and solidification shrinkage. Extensive radial and axial macrosegregation associated with cross-section change is observed. It also appears that steepling and local primary alpha-phase remelting resulting from convection are responsible for stray grain formation at the reentrant corners. Preliminary results from a numerical model, which includes solidification shrinkage and thermosolutal convection in the mushy zone, indicate that these regions are prone to solutal remelting of dendrites.

Ghods, Masoud↗
NASA NTRSDate not supplied

207Pb-206Pb Geochronology and Microstructures of Phosphates From Apollo 14 and 15 Soils

Phosphates (apatite and merrillite) are common accessory minerals in many Apollo basalt and regolith samples. Phosphates typically have lower closure temperatures than their companion accessory phase zircon for their U-Pb and (U-Th)/He geochronologic systems [e.g., 1, 2]. As such, the ages of phosphates in impact melt-bearing breccias have typically been used to constrain the ages of impact events [3]. Phosphates have also served as anchors for 207Pb-206Pb isochrons allowing for precise ages of basaltic samples to be determined [4]. Apatite is also a reservoir for volatile species (e.g., F, Cl, OH, S) [e.g., 5, 6] which are important for investigating the formation and evolution of the lunar interior [7-11]. Recent work by [11] and [12] has shown that deformation and exposure to high temperatures, especially those in impact environments, can influence both apatite chronology and chemistry. Here we present the first chronology and microstructure results of a large consortium study aimed at unraveling the impact and endogenous volatile record of phosphates extracted from lunar soils. These soils potentially sample a larger range of lithologies than the rocks returned by Apollo astronauts, and should, therefore, represent a more global phosphate record. For more information on low temperature (U-Th)/He thermochronology, please see the companion abstract [13].

C A Crow↗
NASA NTRS1999

Use of Microgravity to Control the Microstructure of Eutectics

The long term goal of this project is to be able to control the microstructure of directionally solidified eutectic alloys, through an improved understanding of the influence of convection. Prior experimental results on the influence of microgravity on the microstructure of fibrous eutectics have been contradictory. Theoretical work at Clarkson University showed that buoyancy-driven convection in the vertical Bridgman configuration is not vigorous enough to alter the concentration field in the melt sufficiently to cause a measurable change in microstructure when the eutectic grows at minimum supercooling. Currently, there are four other hypotheses that might explain the observed changes in microstructure of fibrous eutectics caused by convection: (1) Disturbance of the concentration boundary layer arising from an off-eutectic melt composition and growth at the extremum; (2) Disturbance of the concentration boundary layer of a habit-modifying impurity; (3) Disturbance of the concentration boundary layer arising from an off-eutectic interfacial composition due to non-extremum growth; and (4) A fluctuating freezing rate combined with differences in the kinetics of fiber termination and fiber formation. We favor the last of these hypotheses. Thus, the primary objective of the present grant is to determine experimentally and theoretically the influence of a periodically varying freezing rate on eutectic solidification. A secondary objective is to determine the influence of convection on the microstructure of at least one other eutectic alloy that might be suitable for flight experiments.

Wilcox, William R.↗
DOE OSTI2021

Austenite formation and cementite dissolution during intercritical annealing of a medium-manganese steel from a martensitic condition

In the present study, in situ high-energy X-ray diffraction (HEXRD), dilatometry, and metallography were conducted for the purpose of understanding microstructure evolution during intercritical annealing of a Fe-0.19C-4.39Mn steel from a martensitic initial condition. Three different simulations for austenite growth and solute partitioning during isothermal holding were conducted using the DICTRA™ module of Thermo-Calc®. The microstructures after intercritical annealing exhibit film-like retained austenite; however, in situ HEXRD indicates that retained austenite in the initial martensitic microstructure had decomposed upon heating to the isothermal holding temperature, suggesting that film-like austenite may be generated during intercritical annealing via nucleation and growth of new austenite and without necessarily preserving initial retained austenite films in the martensitic microstructure. Metallography and in situ HEXRD also indicate that cementite had formed upon heating but did not readily dissolve during an 1800 s isothermal hold although considerable growth of austenite had occurred during the isothermal hold, suggesting that austenite nucleation and initial growth during intercritical annealing does not solely occur due to carbon partitioning. A simulation incorporating cementite suggests that the increase in austenite fraction during intercritical annealing initially occurs in association with Mn partitioning followed by austenite growth induced by gradual cementite dissolution.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Interface morphology and dislocation-mediated processes during rapid solidification of thin films

Rapid solidification experiments have, in recent years, revealed a wealth of new microstructural phenomena that suggest a strong connection between the kinetics of solidification and the crystalline structures that emerge as a result. In this work, we investigate the interplay between interface morphology and defect-mediated processes during rapid solidification conditions using a Phase Field Crystal (PFC) model, enabling us to simultaneously and efficiently explore the physics of solidification and elasto-plasticity in the formalism of a single-field theory. We predict that there are two mechanisms by which dislocations emitted directly from the solid–liquid interface induce orientation gradients as well as the formation of subgrain boundaries within a single solidifying cell. We relate these mechanisms to the morphology of the moving solid–liquid interface and identify a suitable control parameter in the PFC model with which we can go between said morphologies by effectively changing the relative strength of the capillary length and kinetic coefficients of the solid–liquid interface. Thus, we are able to provide mechanistic explanations for several microstructural features (with an emphasis on orientation gradients and subgrain boundaries) observed during the rapid solidification of pure materials. We also provide a simple explanation for the formation of “jagged” subgrain boundaries, which is consistent with our experimental observations in rapidly solidified samples of Aluminum, whose mechanisms have thus far been unknown.

Interface morphology↗
DOE OSTI2021

Joining AA7099 to Ni-Cr-Mo Steel Using Single Pass Friction Stir Dovetailing and AA6061 Butter Layer

A novel single pass friction stir dovetailing (FSD) was developed to join thick plate AA7099 to Ni-Cr-Mo steel in a lap configuration through the use of an AA6061 butter layer. The butter layer approach can be shown to significantly reduce interfacial failures by inhibiting the formation of brittle Fe–Al intermetallic compounds (IMCs) which are typically formed during conventional friction stir welding (FSW) of AA7099 directly to steel. This study evaluates the strength and microstructural evolution of the aluminum/steel joint interface between single pass FSD of AA7099/AA6061(butter)/steel fabricated using three different FSD tool configurations. The butter layer was achieved by placement of a free-floating strip of AA6061 within the dovetail groove that was pre-machined in the steel substrate. Friction stir welding was then used to simultaneously join the thick plate AA7099, the AA6061 strip and the AA7099 in a single weld pass. To optimize the joining process, three different pin geometries (full thread, half smooth/half thread, no thread) were evaluated; it was demonstrated that the half smooth/half thread tool produced the strongest weld joint due to the absence of a Zn rich layer at the Al/steel interface. The efficacy of this unique processing technique was tested using lap shear tensile testing as well as high resolution transmission electron microscopy (TEM). A discussion of the new FSD technique, joint configurations, and process parameters are provided along with joint microstructural analyses and mechanical performance.

Olszta, Matthew J.↗
DOE OSTI2023

Produced Fluid Induced Mineralogy and Elemental Alterations of Caney Shale, Southern Oklahoma

ABSTRACT This study involves batch reactor experiments and subsequent analyses of samples from Caney Shale in the Ardmore Basin of South-Central Oklahoma. Samples include mainly rock cores and cuttings recovered from two wells respectively drilled vertically through and horizontally across the Caney Shale. Mineralogical compositions are obtained by X-Ray Diffraction (XRD) measurements whilst microstructure and elemental distribution are acquired by Scanning Electron Microscopy/Energy Dispersive Spectroscopy (SEM/EDS) respectively. Batch experiments are then conducted using selected rock samples and produced fluid from the Caney Formation. Deionized water is also reacted with some samples to serve as standard. Experiments are conducted at 95°C and ambient pressure for 7 and 30 days to assess the geochemical rock-fluid interactions. Results show rock mineralogical compositions are predominantly quartz, feldspar, carbonates, and clay with minor pyrite. Post-experimental mineralogical changes observed in samples include increased amorphous entities especially within the clay portions of XRD plots and dissolution of feldspar and carbonate minerals and formation of new mineral phases, mostly clays and salts. These are corroborated by EDS elemental analyses which show decreased elemental compositions. The implications of reactions mentioned above include but not limited to, scale formation, clay fines migration and shale softening all of which pose significant permeability impairment on formation over time. INTRODUCTION Shale reservoirs account for a large share of unconventional reservoirs in the world (Lyu et al., 2015). However, ultra-low permeability and high clay compositions pose significant challenges when producing from these reservoirs (Dawuda and Srinivasan, 2022, 2023). Producing from these reservoirs therefore requires horizontal drilling and hydraulic fracturing technologies which have proven their efficacy in generating substantial permeability in reservoirs to ensure production (Fujian et al., 2019; Liu et al., 2018). Even after expensive horizontal drilling and hydraulic fracturing, geochemical reactions between engineered fluids and formation leads to fracture constriction and adversely impact petrophysical properties (permeability and porosity) of the reservoir. These technologies are therefore under constant development and improvement in various aspects to ensure fine tuning for specific reservoirs. Under present conditions, much of the hydrocarbon reserves in unconventional shale reservoirs are left unproduced due to rapid decline in permeability following resumption to production after hydraulic fracturing. It is therefore essential to understand the range of geochemical reactions that cause rapid depletion of permeability after hydraulic fracturing and apply these to each shale reservoir to ensure substantial recovery rates.

Awejori, G. A.↗
NASA NTRS1985

Rapid solidification characteristics in melt spinning a Ni-base superalloy

The solidification kinetics involved in the process of melt spinning a Ni-base superalloy have been characterized. Through a correlation of ribbon thickness to melt puddle residence time, it was found that the solidification front velocity, V, is typically about 100 mm/sec at the ribbon surface not in contact with the spinning wheel. The rate of solidification varies within the ribbon, increasing with decreasing distance, S, from the wheel-contact surface as V = 3.65/s. Ribbon microstructure and texture characteristics are discussed in light of this kinetics result. The thickness-vs-time correlation was further analyzed to yield information about thermal history during ribbon formation. These thermal results are generally consistent with those deduced from dendrite arm spacing measurements.

Huang, S. C.↗
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↗
NASA NTRS1985

Microstructural aspects of zirconia thermal barrier coatings

Various combination of plasma-sprayed bond coatings and zirconia ceramic coatings on a nickel-based superalloy substrate were tested by static thermal exposure at 1200 C and cyclic thermal exposure to 1000 C. The bond coats were based on Ni-Cr-Al alloys with additions of rare earth elements and Si. The ceramic coats were various ZrO2-Y2O3 compositions, of which the optimum was found to be ZrO2-8.9 wt percent Y2O3. Microstructural analysis showed that resistance to cracking during thermal exposure is strongly related to deleterious phase changes. Zones depleted of Al formed at the bond coat/ceramic coat interface due to oxidation and at the bond coat/substrate interface due to interdiffusion, leading eventually to breakdown of the bond coat. The 8.9 percent Y2O3 coating performed best because the as-sprayed metastable tetragonal phase converted slowly into the low-Y2O3 tetragonal plus high-Y2O3 cubic-phase mixture, so that the deleterious monoclinic phase was inhibited from forming. Failure appeared to start with the formation of circumferential cracks in the zirconia, probably due to compressive stresses during cooling, followed by the formation of radial cracks due to tensile stresses during heating. Cracks appeared to initiate at the Al2O3 scale/bond coat interface and propagate through the zirconia coating. Comparisons were made with the behavior of bulk ZrO2-Y2O3 and the relationship between the microstructure of the tetragonal phase and the phase diagram. A separate investigation was also made of the ZrO2-Al2O3 interface.

Mitchell, T. E.↗
NASA NTRS2012

Solar Ion Sputter Deposition in the Lunar Regolith: Experimental Simulation Using Focused-Ion Beam Techniques

As regions of the lunar regolith undergo space weathering, their component grains develop compositionally and microstructurally complex outer coatings or "rims" ranging in thickness from a few 10 s to a few 100's of nm. Rims on grains in the finest size fractions (e.g., <20 m) of mature lunar regoliths contain optically-active concentrations of nm size metallic Fe spherules, or "nanophase Fe(sup o)" that redden and attenuate optical reflectance spectral features important in lunar remote sensing. Understanding the mechanisms for rim formation is therefore a key part of connecting the drivers of mineralogical and chemical changes in the lunar regolith with how lunar terrains are observed to become space weathered from a remotely-sensed point of view. As interpreted based on analytical transmission electron microscope (TEM) studies, rims are produced from varying relative contributions from: 1) direct solar ion irradiation effects that amorphize or otherwise modify the outer surface of the original host grain, and 2) nanoscale, layer-like, deposition of extrinsic material processed from the surrounding soil. This extrinsic/deposited material is the dominant physical host for nanophase Fe(sup o) in the rims. An important lingering uncertainty is whether this deposited material condensed from regolith components locally vaporized in micrometeorite or larger impacts, or whether it formed as solar wind ions sputtered exposed soil and re-deposited the sputtered ions on less exposed areas. Deciding which of these mechanisms is dominant, or possibility exclusive, has been hampered because there is an insufficient library of chemical and microstructural "fingerprints" to distinguish deposits produced by the two processes. Experimental sputter deposition / characterization studies relevant to rim formation have particularly lagged since the early post-Apollo experiments of Hapke and others, especially with regard to application of TEM-based characterization techniques. Here we report on a novel design for simulating solar ion sputter deposition in the lunar regolith, with characterization of the resulting sputter deposits by an array of advanced analytical TEM techniques.

Christoffersen, R.↗