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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 163 records · Page 9

Heterogeneous doping via nanoscale coating impacts the mechanics of Li intrusion in brittle solid electrolytes

Lithium dendrite intrusion in solid-state batteries limits fast charging and causes short-circuiting, yet the underlying regulating mechanisms are not well-understood. Here, in this work, we discover that heterogeneous Ag + doping dramatically affects lithium intrusion into Li 6.6 La 3 Zr 1.6 Ta 0.4 O 12 (LLZO), a brittle solid electrolyte. Nanoscale Ag + doping is achieved by thermally annealing a 3-nm-thick metallic coating on LLZO, inducing Ag–Li ion exchange and Ag diffusion into grains and grain boundaries. Density functional theory calculations and experimental characterization show negligible impact on the electronic properties and surface wettability from Ag + incorporation. Mechanically, nanoindentation experiments show a fivefold increase in the mechanical force required to fracture the surface Ag + -doped LLZO, indicating substantial doping-induced surface toughening. Operando microprobe scanning electron microscopy experiments show that the Ag + -doped LLZO surface exhibits improved lithium plating at >250 mA cm −2 and an electroplating diameter that is expanded by over fourfold, even under an extreme indentation stress of 3 GPa. This demonstrates enhanced defect tolerance in LLZO, rather than electronic or adhesion effects. Our study reveals a chemo-mechanical mechanism via surface heterogeneous doping, complementing present bulk design rules to minimize mechanical failures in solid-state batteries.

36 MATERIALS SCIENCE↗

Electric field enhanced diffusion welding of alloy 617: Microstructural characteristics and mechanical properties

This study investigated the microstructural characteristics and mechanical behavior of diffusion welded nickel-based Alloy 617 obtained by electric field-assisted sintering (EFAS) using various parameters. The interfacial microstructure exhibited different characteristics including good grain boundary (GB) migration across the interface in the samples diffusion-welded at 1100 °C and a flat interface in the samples joined at 1000 °C and 1050 °C. The interface consisted of fine Al 2 O 3 oxides, while precipitation of interfacial M 23 C 6 carbides was not observed. Grain boundaries migrated across the Al 2 O 3 oxides, leaving these oxides within the grains. Graded grain size was observed, with grain coarsening being more significant near the sample surface due to the temperature gradient induced by EFAS. Tensile testing revealed that the specimens fractured in the matrix away from the interface, indicting strong diffusion-welded joints. Further, the peak tensile strength of 807 MPa was obtained in the samples welded at 1000 °C due to minimal grain growth. The materials obtained at 1100 °C exhibited reduced tensile strength but improved ductility. Strain maps revealed by digital image correlation showed alternating high and low strain segments in the samples produced at 1000 °C and 1050 °C, indicating that the flat interfaces with no GB migration were less ductile compared to the matrix. A greater strain uniformity was observed along the bond interfaces with improved GB migration. The hardness reduced near the sample surfaces due to enlarged grains induced by temperature gradient. This study demonstrates that GB migration and enhanced mechanical strength can be achieved in diffusion-welded Alloy 617.

36 MATERIALS SCIENCE↗

Adhesion, friction, and wear of a copper bicrystal with (111) and (210) grains

Sliding friction experiments were conducted in air with polycrystalline copper and ruby riders sliding against a copper bicrystal. Friction coefficient was measured across the bicrystal surface, and the initiation of adhesive wear was examined with scanning electron microscopy. Results indicate a marked increase in friction coefficient as the copper rider crossed the grain boundary from the (111) plane to the (210) plane of the bicrystal. Adhesion, friction, and initiation of adhesive wear was notably different in the adjacent grains of differing orientation. A slip-band adhesion-generated fracture mechanism for wear particle formation is proposed.

Brainard, W. A.↗

Mechanisms of devitrification of grain boundary glassy phases in Si3N4 materials

Changes in the grain boundary (g.b.) phases of Si3N4 are analyzed, the effects of composition and thermal history on devitrification of the g.b. phases are determined, devitrification of the g.b. phases of Si3N are related to mechanical behavior and oxidation sensitivity of the material. The phase relationships that occur within the grain boundaries of Si3N4 containing various densification aids are reviewed. Comparisons of the effects of MgO, Y2O3, CeO2, and Y2O3 + AL2O3 are made in terms of the phase equilibria of the Si3N4 + SiO2 + additive compositional system. Two new equilibrium phase diagrams for the Si3N4-SiO2 and Y2O3 and Si3N4-SiO2-Ce2O3 systems are preented. The effects of Y2O3 vs CeO2 densification aids on the fracture surfaces of Si3N4 are compared. Auger electron spectroscopy shows that both oxides are concentrated within the fracture surface. Scanning electron microscopy shows evidence that Si3N4 with CeO2 formed an intergranular structure of fine grained oxynitride reaction products, as predicted by phase quilibria, whereas the Y2O3 containing sample shows evidence of an intergranular glassy phase.

Hench, L. L.↗

Multiscale Thermomechanical Damage Model with Internal State Variables for Ceramic Matrix Composites

A length scale-dependent matrix damage model has been developed to simulate the response of ceramic matrix composites (CMCs). This model captures damage initiation and propagation in the brittle matrix material by employing internal state variable (ISV) theory within a multiscale modeling framework to obtain damaged matrix stress-strain constitutive relationships at each length scale. Material degradation due to matrix cracking is captured by a damage variable determined using fracture mechanics and the self-consistent scheme. An additional state variable is introduced to capture the nucleation and growth of matrix porosity, a key mechanism contributing to matrix nonlinearity. Porosity occurs as a result of material diffusion around grain boundaries and the growth of the porosity state variable is related to the material entropy dissipation and the volumetric strain. The nonlinear predictive capabilities of the material model are demonstrated for monolithic silicon carbide, unidirectional (UD) carbon fiber/silicon carbide matrix (C/SiC) CMC, and five-harness satin (5HS) woven C/SiC CMC.

Skinner, Travis D.↗

Microstructural Characteristics, Mechanical Properties, and Corrosion Behavior of Field-Assisted Diffusion Welded Alloy 617

This study investigated the microstructural characteristics, mechanical response, and corrosion resistance of Alloy 617 diffusion welded by electric field-assisted sintering (EFAS). The microstructure exhibited good grain boundary (GB) migration across the interface and flat interface in the samples bonded at different conditions. Graded grain size was observed, with grain coarsening being more significant near sample surface due to EFAS-induced temperature gradient. Tensile testing revealed that the specimens fractured in the matrix away from the interface. The peak strength of 807 MPa was obtained in the samples welded at 1000°C. The materials obtained at 1100°C exhibited reduced tensile strength but improved ductility. Strain maps revealed by digital image correlation showed the flat interfaces were less ductile compared to the matrix. The hardness reduced near sample surfaces due to enlarged grains induced by temperature gradient. The interfaces with GB migration exhibited improved corrosion resistance in molten salt compared to the flat interfaces.

36 - MATERIALS SCIENCE↗

Elevated temperature crack growth in advanced powder metallurgy aluminum alloys

Rapidly solidified Al-Fe-V-Si powder metallurgy alloy FVS0812 is among the most promising of the elevated temperature aluminum alloys developed in recent years. The ultra fine grain size and high volume fraction of thermally stable dispersoids enable the alloy to maintain tensile properties at elevated temperatures. In contrast, this alloy displays complex and potentially deleterious damage tolerant and time dependent fracture behavior that varies with temperature. J-Integral fracture mechanics were used to determine fracture toughness (K sub IC) and crack growth resistance (tearing modulus, T) of extruded FVS0812 as a function of temperature. The alloy exhibits high fracture properties at room temperature when tested in the LT orientation, due to extensive delamination of prior ribbon particle boundaries perpendicular to the crack front. Delamination results in a loss of through thickness constraint along the crack front, raising the critical stress intensity necessary for precrack initiation. The fracture toughness and tensile ductility of this alloy decrease with increasing temperature, with minima observed at 200 C. This behavior results from minima in the intrinsic toughness of the material, due to dynamic strain aging, and in the extent of prior particle boundary delaminations. At 200 C FVS0812 fails at K levels that are insufficient to cause through thickness delamination. As temperature increases beyond the minimum, strain aging is reduced and delamination returns. For the TL orientation, K (sub IC) decreased and T increased slightly with increasing temperature from 25 to 316 C. Fracture in the TL orientation is governed by prior particle boundary toughness; increased strain localization at these boundaries may result in lower toughness with increasing temperature. Preliminary results demonstrate a complex effect of loading rate on K (sub IC) and T at 175 C, and indicate that the combined effects of time dependent deformation, environment, and strain aging may play a role. Fractography showed that microvoid coalescence was the microscopic mode of fracture in FVS0812 under all testing conditions. However, the nature of the microvoids varied with test temperature and loading rate, and is complex for the fine grain and dipersoid sizes of FVS0812.

Porr, William C., Jr.↗

Intergranular fracture of lithium fluoride-22 percent calcium fluoride hypereutectic salt at 800 K

Substantial strain-hardening was noted during the initial stages of deformation in constant-velocity compression tests conducted on as-cast samples of the LiF-22 mol pct CaF2 hypereutectic salt at 800 K. The deformed specimens exhibited extensive grain-boundary cracking and cavitation, suggesting that such cracking, in conjunction with interfacial sliding, is important for cavity nucleation at grain boundaries and at the LiF-CaF2 interfaces. Cavity growth and interlinkage occur through the preferential failure of the weaker LiF phase.

Raj, Subramanium V.↗

Mechanism of slip and twinning

The objectives are to: (1) demonstrate the mechanisms of deformation in body centered cubic (BCC), face centered cubic (FCC), and hexagonal close-packed (HCP)-structure metals and alloys and in some ceramics as well; (2) examine the deformed microstructures (slip lines and twin boundaries) in different grains of metallic and ceramic specimens; and (3) study visually the deformed macrostructure (slip and twin bands) of metals and alloys. Some of the topics covered include: deformation behavior of materials, mechanisms of plastic deformation, slip bands, twin bands, ductile failure, intergranular fracture, shear failure, slip planes, crystal deformation, and dislocations in ceramics.

Rastani, Mansur↗

Separating the Influence of Environment from Stress Relaxation Effects on Dwell Fatigue Crack Growth in a Nickel-Base Disk Alloy

Both environmental embrittlement and crack tip visco-plastic stress relaxation play a significant role in determining the dwell fatigue crack growth (DFCG) resistance of nickel-based disk superalloys. In the current study performed on the Low Solvus High Refractory (LSHR) disk alloy, the influence of these two mechanisms were separated so that the effects of each could be quantified and modeled. Seven different microstructural variations of LSHR were produced by controlling the cooling rate and the subsequent aging and thermal exposure heat treatments. Through cyclic fatigue crack growth testing performed both in air and vacuum, it was established that four out of the seven LSHR heat treatments evaluated, possessed similar intrinsic environmental resistance to cyclic crack growth. For these four heat treatments, it was further shown that the large differences in dwell crack growth behavior which still persisted, were related to their measured stress relaxation behavior. The apparent differences in their dwell crack growth resistance were attributed to the inability of the standard linear elastic fracture mechanics (LEFM) stress intensity parameter to account for visco-plastic behavior. Crack tip stress relaxation controls the magnitude of the remaining local tensile stresses which are directly related to the measured dwell crack growth rates. It was hypothesized that the environmentally weakened grain boundary crack tip regions fail during the dwells when their strength is exceeded by the remaining local crack tip tensile stresses. It was shown that the classical creep crack growth mechanisms such as grain boundary sliding did not contribute to crack growth, but the local visco-plastic behavior still plays a very significant role by determining the crack tip tensile stress field which controls the dwell crack growth behavior. To account for the influence of the visco-plastic behavior on the crack tip stress field, an empirical modification to the LEFM stress intensity parameter, Kmax, was developed by incorporating into the formulation the remaining stress level concept as measured by simple stress relaxation tests. The newly proposed parameter, Ksrf, did an excellent job in correlating the dwell crack growth rates for the four heat treatments which were shown to have similar intrinsic environmental cyclic fatigue crack growth resistance.

Dwell crack growth↗

Separating the Influence of Environment from Stress Relaxation Effects on Dwell Fatigue Crack Growth

Seven different microstructural variations of LSHR were produced by controlling the cooling rate and the subsequent aging and thermal exposure heat treatments. Through cyclic fatigue crack growth testing performed both in air and vacuum, it was established that four out of the seven LSHR heat treatments evaluated, possessed similar intrinsic environmental resistance to cyclic crack growth. For these four heat treatments, it was further shown that the large differences in dwell crack growth behavior which still persisted, were related to their measured stress relaxation behavior. The apparent differences in their dwell crack growth resistance were attributed to the inability of the standard linear elastic fracture mechanics (LEFM) stress intensity parameter to account for visco-plastic behavior. Crack tip stress relaxation controls the magnitude of the remaining local tensile stresses which are directly related to the measured dwell crack growth rates. It was hypothesized that the environmentally weakened grain boundary crack tip regions fail during the dwells when their strength is exceeded by the remaining local crack tip tensile stresses. It was shown that the classical creep crack growth mechanisms such as grain boundary sliding did not contribute to crack growth, but the local visco-plastic behavior still plays a very significant role by determining the crack tip tensile stress field which controls the dwell crack growth behavior. To account for the influence of the visco-plastic behavior on the crack tip stress field, an empirical modification to the LEFM stress intensity parameter, Kmax, was developed by incorporating into the formulation the remaining stress level concept as measured by simple stress relaxation tests. The newly proposed parameter, Ksrf, did an excellent job in correlating the dwell crack growth rates for the four heat treatments which were shown to have similar intrinsic environmental cyclic fatigue crack growth resistance.

environmental damage↗

Relation of cyclic loading pattern to microstructural fracture in creep fatigue

Creep-fatigue-environment interaction is discussed using the 'strainrange partitioning' (SRP) framework as a basis. The four generic SRP strainrange types are studied with a view of revealing differences in micromechanisms of deformation and fatigue degradation. Each combines in a different manner the degradation associated with slip-plane sliding, grain-boundary sliding, migration, cavitation, void development and environmental interaction; hence the approch is useful in delineating the relative importance of these mechanisms in the different loadings. Micromechanistic results are shown for a number of materials, including 316 SS, wrought heat resistant alloys, several nickel-base superalloys, and a tantalum base alloy, T-111. Although there is a commonality of basic behavior, the differences are useful in delineation several important principles of interpretation. Some quantitative results are presented for 316 SS, involving crack initiation and early crack growth, as well as the interaction of low-cycle fatigue with high-cycle fatigue.

Manson, S. S.↗

Microscale mechanical property variations of Al-substituted LLZO: insights from compression testing and molecular dynamics simulations

Ceramic solid electrolytes based on LLZO (Li 7 La 3 Zr 2 O 12 ) are promising candidates for all-solid-state batteries due to their high ionic conductivity and good apparent stability vs. lithium metal, however they are prone to mechanical failure. Lithium metal intrusions, alongside cell stack pressure, transition polycrystalline solid electrolyte grains into a compressed state that promotes crack propagation and fracture. Here this work examines the mechanical response of Al-substituted LLZO to compressive forces by measuring ultimate strength under pillar compression with a flat punch tip. Failure modes characterized by in situ scanning electron microscopy show diverse splitting patterns arising from internal porosity, grain boundaries, and slip planes. Large correlated variations in compressive strength (0.93–2.63 GPa) and Young's modulus (72.1–150.97 GPa) are observed across microscale regions of the solid electrolyte. Molecular dynamics simulations of LLZO with different porosities describe the variation of compressive strength and Young's modulus, and enable a microscale porosity model to be fit accounting for Young's modulus reduction across the solid electrolyte. Overall, the results indicate the importance of microscale mechanical testing of ceramic solid electrolytes to identify preferential sites for mechanical degradation and Li intrusion, and ensure the robust design of all-solid-state lithium metal batteries.

25 ENERGY STORAGE↗

Metallurgical Mechanisms Controlling Mechanical Properties of Aluminum Alloy 2219 Produced by Electron Beam Freeform Fabrication

The electron beam freeform fabrication (EBF3) layer-additive manufacturing process has been developed to directly fabricate complex geometry components. EBF3 introduces metal wire into a molten pool created on the surface of a substrate by a focused electron beam. Part geometry is achieved by translating the substrate with respect to the beam to build the part one layer at a time. Tensile properties demonstrated for electron beam deposited aluminum and titanium alloys are comparable to wrought products, although the microstructures of the deposits exhibit cast features. Understanding the metallurgical mechanisms controlling mechanical properties is essential to maximizing application of the EBF3 process. Tensile mechanical properties and microstructures were examined for aluminum alloy 2219 fabricated over a range of EBF3 process variables. Unique microstructures were observed within the deposited layers and at interlayer boundaries, which varied within the deposit height due to microstructural evolution associated with the complex thermal history experienced during subsequent layer deposition. Microstructures exhibited irregularly shaped grains with interior dendritic structures, described based on overall grain size, morphology, distribution, and dendrite spacing, and were correlated with deposition parameters. Fracture features were compared with microstructural elements to define fracture paths and aid in definition of basic processing-microstructure-property correlations.

Domack, Marcia S.↗

Metallurgical Design and Development of NASA Crawler/Transporter Tread Belt Shoe Castings

The NASA Crawler/Transporters (CT-1 and CT-2) used to transport the Space Shuffles are one of the largest tracked vehicles in existence today. Two of these machines have been used to move space flight vehicles at Kennedy Space Center since the Apollo missions of the 1960's and relatively few modifications have been made to keep them operational. In September of 2003 during normal Crawler/Transporter operations cracks were observed along the roller pad surfaces of several tread belt shoes. Further examination showed 20 cracked shoes on CT-1 and 40 cracked shoes on CT-2 and a formal failure analysis investigation was undertaken while the cracked shoes were replaced. Six shoes were cross-sectioned with the fracture surfaces exposed and it was determined that the cracks were due to fatigue that initiated on the internal casting web channels at pre-existing casting defects and propagated through thickness both transgranularly and intergranularly between internal shrinkage cavities, porosity, and along austenitic and ferritic grain boundaries. The original shoes were cast during the 1960's using a modified 861330 steel with slightly higher levels of chromium, nickel and molybdenum followed by heat treatment to achieve a minimum tensile strength of 11 Oksi. Subsequent metallurgical analysis of the tread belt shoes after multiple failures showed excessive internal defects, alloy segregation, a nonuniform ferritic/ bainitic/martensitic microstructure, and low average tensile properties indicative of poor casting and poor heat-treatment. As a result, NASA funded an initiative to replace all of the tread belt shoes on both crawler/transporters along with a redesign of the alloy, manufacturing, and heat-treatment to create a homogeneous cast structure with uniform mechanical and metallurgical properties. ME Global, a wholly owned subsidiary of ME Elecmetal based in Minneapolis, MN was selected as manufacturing and design partner to develop the new shoes and this paper describes the research, development, and manufacturing that resulted in the successful delivery of 1044 new Crawler/Transporter tread belt shoes all meeting rigid metallurgical and mechanical design criteria derived from finite element modeling of the stress loads required for safe space shuttle transport.

Parker, Donald S.↗

Mechanical behavior of polycrystalline ceramics: Brittle fracture of SiC-Si3N4 materials

Various properties of ceramic materials were investigated. Magnesium oxide and the role of anion impurities were investigated together with the slow crack growth in silicon nitride-silicon carbide ceramics. The oxide program involved development of fabrication techniques for anion doped materials and evaluation of the role of these anions in the hot pressing response, grain boundary diffusion of nickel doped material, grain boundary microhardness, and grain growth. The carbide-nitride work employed commercial materials and the research involved evaluation of a recently reported technique for study of slow crack growth and the development of data for these commercial materials.

Leipold, M. H.↗

Mechanical behavior of polycrystalline ceramics: Brittle fracture of SiC-Si3N4 materials

The first study area involved magnesium oxide and the role of anion impurities, while the second area was directed toward slow crack growth in silicon nitride-silicon carbide ceramics. The oxide program involved development of fabrication techniques for anion doped materials and evaluation of the role of these anions in the hot pressing response, grain boundary diffusion of nickel doped material, grain boundary microhardness, and grain growth.

Leipold, M. H.↗