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DOE OSTI2026

Chemo-Mechanics of α-V 2 O 5 During Lithiation and Implications for Rechargeable Battery Cathodes

Chemo-mechanical degradation of layered oxide electrodes is strongly influenced by crystallographic anisotropy, local stress evolution, and ion insertion, yet the intrinsic mechanical response of layered materials remains incompletely understood. Indeed, most prior studies have focused on polycrystalline materials but single crystals enable direct observation of coupling between anisotropic ion diffusion and mechanical response. This study aims to determine how crystallographic anisotropy and lithiation affect deformation, fracture, and mechanical properties in single-crystal V 2 O 5 , and compares this behavior with polycrystalline counterparts. Polycrystalline V 2 O 5 thin films and single-crystal α-V 2 O 5 were studied using nanoindentation, scanning electron microscopy, focused ion beam cross-sectioning, and Raman spectroscopy. Single crystals were tested in pristine and chemically lithiated states, including experiments in which crystals were first plastically deformed via nanoindentation and subsequently lithiated. Polycrystalline films exhibited significantly higher hardness and elastic modulus than single crystals. Single crystals indented normal to the exposed (001) basal plane exhibited pronounced anisotropic deformation, including directional slip, crystallographically-guided cracking, anisotropic crack propagation, interlayer separation, and shear localization. Lithiation caused substantial softening, reduced hardness and modulus, and suppressed displacement bursts during nanoindentation, while previously indented regions showed crack formation and growth upon lithiation. Mechanical behavior of α-V 2 O 5 is strongly governed by crystallographic anisotropy and further altered by lithiation, with pre-existing deformation serving as a strong driver of fracture during ion insertion. These findings illuminate the coupling among ion insertion, deformation, and fracture in layered oxides and provide a basis for understanding and mitigating mechanical failure in electrochemical energy-storage materials.

Anisotropy↗

NASA NTRS2002

Origin of Magnetic Lineations on Mars

The magnetic lineations discovered by MGS (Mars Global Surveyor) have been considered to be evidence of early plate tectonics on Mars. However, the lineations approximately follow lines of latitude, i.e., small circles. This presents significant geometrical problems for plate-like spreading, particularly at high latitudes. However, the sublatitudinal orientation of the lineations is consistent with meridianal extension and perhaps limited crustal spreading due to a stress event centered near the geographic pole. We hypothesize that this event was the early formation of the crustal dichotomy through mantle-convective processes. This could have taken the form of a southern megaplume that formed the thick highlands crust or as subduction or downwelling in the north. Both would result in tensional stresses in the south that would form extensional fractures perpendicular to the CM-CF (center-of-mass/center-of-gravity) offset. The observed magnitude and distribution of magnetization indicates that crustal intrusion associated with this major mantle-convective event resulted in approximately 1000 km of extension in the Southern highlands. Subsequent spin-axis reorientation due to loss of crust in the north or gain of crust in the south brought the CM-CF offset into its present N-S alignment. A portion of the ancient valley networks observed in the southern highlands are spatially associated with crustal magnetism and are quantitatively shown to be consistent with hydrothermal discharge over crustal intrusions.

Grimm, Robert E.↗

NASA NTRS1987

A micrographic study of bending failure in five thermoplastic/carbon fiber composite laminates

The local deformation and failure sequences of five thermoplastic matrix composites were microscopically observed while bending the samples in a small fixture attached to a microscope stage. The themoplastics are polycarbonate, polysulfone, polyphenylsulfide, polyethersulfone, and polyetheretherketone. Comparison was made to an epoxy matrix composite, 5208/T-300. Laminates tested are (0/90) sub 2S, with outer ply fibers parallel to the beam axis. Four point bending was used at a typical span-to-thickness ratio of 39:1. It was found that all of the thermoplastic composites failed by abrupt longitudinal compression buckling of the outer ply. Very little precursory damage was observed. Micrographs reveal typical fiber kinking associated with longitudinal compression failure. Curved fracture surfaces on the fibers suggest they failed in bending rather than direct compression. Delamination was suppressed in the thermoplastic composites, and the delamination that did occur was found to be the result of compression buckling, rather than visa-versa. Microbuckling also caused other subsequent damage such as ply splitting, transverse ply shear failure, fiber tensile failure, and transverse ply cracking.

Yurgartis, S. W.↗

NASA NTRS1988

A micrographic study of bending failure in five thermoplastic-carbon fibre composite laminates

The local deformation and failure sequences of five thermoplastic matrix composites were microscopically observed while bending the samples in a small fixture attached to a microscope stage. The thermoplastics are polycarbonate, polysulfane, polyphenylsulfide, polyethersulfane, and polyetheretherketone. Comparison was made to an epoxy matrix composite, 5208/T-300. Laminates tested are (0/90) sub 2S, with outer ply fibers parallel to the beam axis. Four point bending was used at a typical span-to-thickness ratio of 39:1. It was found that all of the thermoplastic composites failed by abrupt longitudinal compression buckling of the outer ply. Very little precursory damage was observed. Micrographs reveal typical fiber kinking associated with longitudinal compression failure. Curved fracture surfaces on the fibers suggest they failed in bending rather than direct compression. Delamination was suppressed in the thermoplastic composites, and the delamination that did occur was found to be the result of compression buckling, rather than vice-versa. Microbuckling also caused other subsequent damage such as ply splitting, transverse ply shear failure, fiber tensile failure, and transverse ply cracking.

Yurgartis, S. W.↗

NASA NTRS1994

Assessment of antipodal-impact terrains on Mars

The regions anitpodal to Mars' three largest impact basins, Hellas, Isidis, and Argyre, were assessed for evidence of impact-induced disrupted terrains. Photogeology and computer modeling using the Simplified Arbitrary Lagrangian Eulerian (SALE) finite element code suggest that such terrains could have been found by the Hellas impact. Maximum antipodal pressures are 1100 MPa for Hellas, 520 MPa for Isidis, and 150 MPa for Argyre. The results suggest that if antipodal fracturing were associated with later volcanism, then Alba Patera may be related to the Hellas event, as proposed by Peterson (1978). Alba Patera is a unique volcano in the solar system, being a shield volcano which emitted large volume lava flows. This volcanism could be the result of the focusing of seismic energy which created a fractured region that served as a volcanic conduit for the future release of large volumes of magma. No disrupted terrain features are observed antipodal to the Isidis or Argyre basins, although some of the old fractures in Noctis Labyrinthus could have originated in response to the Isidis impact, and later have been reactivated by the Tharsis tectonics assumed to have produced Noctis. If the lower calculated antipodal pressures for Argyre were capable of producing disrupted terrains, then the terrains have been covered subsequently by volcanic or aeolian material, or modified beyond recognition.

Williams, David A.↗

DOE OSTI2025

Investigation of Solid Particle Reactors for Nonoxidative Dehydrogenation of Ethane: Toward Solar Thermal Ethylene Production

Concentrating solar power plants can generate renewable heat at temperatures well above those of most industrial processes. Ceramic particles irradiated with concentrated sunlight can store high-quality sensible heat and transfer this to power generation systems. These concepts and materials hold great potential to also enable thermal processes in the chemical industry, but effective strategies for transferring heat from thermal energy storage media into chemical reactors are still under development. This present work evaluated the thermal and chemical compatibility of various solid particle media (including quartz, bauxite, and alumina particles) integrated directly into tube reactors and the subsequent effects on reactor performance for the nonoxidative dehydrogenation of ethane reaction. Empty tube reactors without loaded particles (representing conventional ethane cracking coils) showed significant heat transfer limitations as the tube diameter was scaled. The incorporation of media into the reactor significantly aided heat transfer to the gaseous ethane reactant and increased its conversion by as much as 10% at similar space velocities. Despite direct contact with hydrocarbon gases, alumina and quartz media showed negligible coke formation. Even during reaction in 100% ethane feed gas at 825 °C, the average selectivity of the coke product was only 0.57% when using the quartz media. These materials further demonstrated excellent thermal stability during subsequent reoxidation in air at 800 °C, which simulated the reheating of particles in a circulating particle solar receiver. Conversely, high rates of coke formation, with a product selectivity of 27.5%, were observed on sintered bauxite particles during the reaction, likely promoted by transition metal constituents. These particles fractured upon reoxidation due to exotherms generated from coke combustion. In conclusion, while the use of cofed steam could mitigate attrition of redox-active particles, the ability of inert metal oxide particles to efficiently transfer heat to concentrated ethane reactant gas while suppressing side reactions or degradation suggests that these media could effectively couple solar thermal plants to reactors for next-generation production of ethylene and other critical chemicals.

Hydrocarbons↗

NASA NTRS1995

Low Cost Fabrication of Silicon Carbide Based Ceramics and Fiber Reinforced Composites

A low cost processing technique called reaction forming for the fabrication of near-net and complex shaped components of silicon carbide based ceramics and composites is presented. This process consists of the production of a microporous carbon preform and subsequent infiltration with liquid silicon or silicon-refractory metal alloys. The microporous preforms are made by the pyrolysis of a polymerized resin mixture with very good control of pore volume and pore size thereby yielding materials with tailorable microstructure and composition. Mechanical properties (elastic modulus, flexural strength, and fracture toughness) of reaction-formed silicon carbide ceramics are presented. This processing approach is suitable for various kinds of reinforcements such as whiskers, particulates, fibers (tows, weaves, and filaments), and 3-D architectures. This approach has also been used to fabricate continuous silicon carbide fiber reinforced ceramic composites (CFCC's) with silicon carbide based matrices. Strong and tough composites with tailorable matrix microstructure and composition have been obtained. Microstructure and thermomechanical properties of a silicon carbide (SCS-6) fiber reinforced reaction-formed silicon carbide matrix composites are discussed.

Singh, M.↗

NASA NTRS2012

Elastic Plastic Fracture Analysis of an Aluminum COPV Liner

Onboard any space-launch vehicle, composite over-wrapped pressure vessels (COPVs) may be utilized by propulsion or environmental control systems. The failure of a COPV has the potential to be catastrophic, resulting in the loss of vehicle, crew or mission. The latest COPV designs have reduced the wall-thickness of the metallic liner to the point where the material strains plastically during operation. At this time, the only method to determine the damage tolerance lifetime (safe-life) of a plastically responding metallic liner is through full-scale COPV testing. Conducting tests costs substantially more and can be far more time consuming than performing an analysis. As a result of this cost, there is a need to establish a qualifying process through the use of a crack growth analysis tool. This paper will discuss fracture analyses of plastically responding metallic liners in COPVs. Uni-axial strain tests have been completed on laboratory specimens to collect elastic-plastic crack growth data. This data has been modeled with the crack growth analysis tool, NASGRO 6.20 to predict the response of laboratory specimens and subsequently the complexity of a COPV.

Forth, Scott↗

NASA NTRS1984

Rapidly solidified NiAl and FeAl

Melt spinning was used to produce rapidly solidified ribbons of the B2 intermetallics NiAl and FeAl. Both Fe-40Al and Fe-45Al possessed some bend ductility in the as spun condition. The bend ductility of Fe-40Al, Fe-45Al, and equiatomic NiAl increased with subsequent heat treatment. Heat treatment at approximately 0.85 T (sub m) resulted in significant grain growth in equiatomic FeAl and in all the NiAl compositions. Low bend ductility in both FeAl and NiAl generally coincided with intergranular failure, while increased bend ductility was characterized by increasing amounts of transgranular cleavage fracture.

Gaydosh, D. J.↗

NASA NTRS1985

Rapidly solidified NiAl and FeAl

Gaydosh, D. J.↗

DOE OSTI2024

Optimal Geometry for Focused Ion Beam-Milled Samples for Direct-Pull Micro-Tensile Testing Performed In Situ in a Scanning Electron Microscope

A thorough procedure was developed to efficiently manufacture dogbone samples using focused ion beam (FIB) milling for micro-tensile testing. A Bruker PI 89 PicoIndenter, Billerica, MA, USA, was used as a case study, although the analysis and results are applicable to other micro-mechanical testing systems capable of mounting a standard, Ø12.7 mm × Ø3.2 mm pin, scanning electron microscopy (SEM) pin stub (Ted Pella, Redding, CA, USA). Nine dogbones were made from an Fe-45Cu alloy additively manufactured using powder-fed laser-directed energy deposition (DED-LB). Testing showed that fracture was confined to the gauge section for all dogbones and that the fracture mode, ductile vs. brittle, was entirely dependent on the grain orientation relative to the loading direction. The analysis showed that the measured plastic strain to failure can vary from >11% (optimal geometry) to <1% (non-optimal geometry) in micro-tensile testing of high-tensile-strength (>1 GPa) metallic materials. Subsequently, a finite element analysis (FEA) was conducted to identify the improved dogbone geometries. A total of ten thousand dogbone geometries were tested, and their dimensions were defined by a set of four adjustable parameters (corner radius, load surface angle, load surface length, and dogbone head length). The gauge width and gauge length were fixed to 4 µm and 10 µm, respectively. Three-dimensional surface plots of the stress concentration as a function of two parameters were used to identify the optimal ranges of parameter values. The addition of maximum width and length constraints, measuring 25 µm and 30 µm, respectively, allowed us to identify an optimal geometry at load surface angles of 30° and 45°. Their respective dimensions (corner radius, load surface length, and dogbone head length) are, in µm, 12, 6, and 7 and 10, 7, and 7. Testing these two optimal geometries with a range of gauge lengths from 4 to 20 µm showed that smaller gauge lengths only slightly reduced the detrimental stress concentration outside the gauge section. However, smaller gauge lengths will notably improve the FIB surface polishing step as tapering is reduced with smaller dogbone lengths.

Chemistry↗

NASA NTRS1991

Local delamination in laminates with angle ply matrix cracks. Part 2: Delamination fracture analysis and fatigue characterization

Constant amplitude tension-tension fatigue tests were conducted on AS4/3501-6 graphite/epoxy (02/ theta sub 2/ -(theta sub 2))sub s laminates, where theta was 15, 20, 25, or 30 degrees. Fatigue tests were conducted at a frequency of 5 Hz and an R-ratio of 0.1. Dye penetrant enhanced x-radiography was used to document the onset of matrix cracking in the central -(theta) degree plies, and the subsequent onset of local delaminations in the theta/ -(theta) interface at the intersection of the matrix cracks and the free edge, as a function of the number of fatigue cycles. Two strain energy release rate solutions for local delamination from matrix cracks were derived: one for a local delamination growing from an angle ply matrix crack with a uniform delamination growing from an angle ply matrix crack with a triangular shaped delamination area that extended only partially into the laminate width from the free edge. Plots of G(max) vs. N were generated to assess the accuracy of these G solutions. The influence of residual thermal and moisture stresses on G were also quantified. However, a detailed analysis of the G components and a mixed-mode fatigue failure criterion for this material may be needed to predict the fatigue behavior of these laminates.

Obrien, T. Kevin↗

NASA NTRS2014

Gale Crater and Impact Processes - Curiosity's First 364 Sols on Mars

Impact processes at all scales have been involved in the formation and subsequent evolution of Gale crater. Small impact craters in the vicinity of the Curiosity MSL landing site and rover traverse during the 364 Sols after landing have been studied both from orbit and the surface. Evidence for the effect of impacts on basement outcrops may include loose blocks of sandstone and conglomerate, and disrupted (fractured) sedimentary layers, which are not obviously displaced by erosion. Impact ejecta blankets are likely to be present, but in the absence of distinct glass or impact melt phases are difficult to distinguish from sedimentary/volcaniclastic breccia and conglomerate deposits. The occurrence of individual blocks with diverse petrological characteristics, including igneous textures, have been identified across the surface of Bradbury Rise, and some of these blocks may represent distal ejecta from larger craters in the vicinity of Gale. Distal ejecta may also occur in the form of impact spherules identified in the sediments and drift material. Possible examples of impactites in the form of shatter cones, shocked rocks, and ropy textured fragments of materials that may have been molten have been observed, but cannot be uniquely confirmed. Modification by aeolian processes of craters smaller than 40 m in diameter observed in this study, are indicated by erosion of crater rims, and infill of craters with aeolian and airfall dust deposits. Estimates for resurfacing suggest that craters less than 15 m in diameter may represent steady state between production and destruction. The smallest candidate impact crater observed is ∼0.6 m in diameter. The observed crater record and other data are consistent with a resurfacing rate of the order of 10 mm/Myr; considerably greater than the rate from impact cratering alone, but remarkably lower than terrestrial erosion rates.

Curiosity↗

NASA NTRS2000

Aging Effects of Environmentally-Friendly Cleaners on Adhesive Bond Integrity

Because of the 1990 Clean Air Act Amendment many chlorinated solvents are being phased out of use in manufacturing industries. Replacement of the ODC (ozone- depleting chemicals) with less volatile, non-ozone depleting cleaners has been extensively studied over the past nine years at Thiokol Propulsion, Cordant Technologies. Many of the non-ODC cleaners contain compounds that can potentially degrade over time under conditions of high temperature, humidity and exposure to light. The chemical composition of environmentally conditioned cleaners and the subsequent effect on aluminum/amine-cured epoxy bond integrity as measured by Tapered Double Cantilever Beam were evaluated. From this study it is observed that moisture content increases for those cleaners containing polar compounds. Non-volatile residue content increases as stabilizers are depleted and the chemical compound limonene is oxidized. A change in aluminum/ amine-cured epoxy bond fracture toughness is observed as some of these cleaners age with increases in moisture and NVR content.

Biegert, L. L.↗

NASA NTRS1986

On fracture of fibrous composites

The problem of an existing through-the-thickness center notch in a unidirectional fibrous composite is investigated using a homogeneous anisotropic elasticity analysis in conjunction with various crack growth criteria. Tensor polynomial, strain energy density, and normal stress ratio criteria are applied as crack growth direction criteria and compared to experimental observations. For the cases and criteria studied, only the normal stress ratio criterion exhibits an ability to correctly predict crack growth direction. The normal stress ratio criterion is subsequently applied to the same cases as a failure criterion. Comparison with experiment indicates that these predictions exhibit reasonable correlation with observed critical stresses. Finally, the macroscopic approach to the problem used in this study is compared to a microscopic shear lag analysis of experimental results in the literature. The comparison indicates that both approaches yield essentially identical predictions. The comparisons made with other criteria and approaches indicate that application of the normal stress ratio within a macroscopic level analysis has great potential as an approach to modeling composite crack growth.

Beuth, J. L., Jr.↗

NASA NTRS1994

Investigation of failure to separate an Inconel 718 frangible nut

The 2.5-inch frangible nut is used in two places to attach the Space Shuttle Orbiter to the External Tank. It must be capable of sustaining structural loads and must also separate into two pieces upon command. Structural load capability is verified by proof loading each flight nut, while ability to separate is verified on a sample of a production lot. Production lots of frangible nuts beginning in 1987 experienced an inability to reliably separate using one of two redundant explosive boosters. The problems were identified in lot acceptance tests, and the cause of failure has been attributed to differences in the response of the Inconel 718. Subsequent tests performed on the frangible nuts resulted in design modifications to the nuts along with redesign of the explosive booster to reliably separate the frangible nut. The problem history along with the design modifications to both the explosive booster and frangible nut are discussed in this paper. Implications of this failure experience impact any pyrotechnic separation system involving fracture of materials with respect to design margin control and lot acceptance testing.

Hoffman, William C., III↗

NASA NTRS1975

Seismic effects from major basin formations on the moon and Mercury

Grooved and hilly terrains occur at the antipode of major basins on the moon (Imbrium, Orientale) and Mercury (Caloris). Such terrains may represent extensive landslides and surface disruption produced by impact-generated P-waves and antipodal convergence of surface waves. Order-of-magnitude calculations for an Imbrium-size impact on the moon indicate P-wave-induced surface displacements of 10 m at the basin antipode that would arrive prior to secondary ejecta. Comparable surface waves would arrive subsequent to secondary ejecta impacts beyond 1000 km and would increase in magnitude as they converge at the antipode. Other seismically induced surface features include: subdued, furrowed crater walls produced by landslides and concomitant secondary impacts; emplacement and leveling of light plains units owing to seismically induced 'fluidization' of slide material; and perhaps the production and enhancement of deep-seated fractures that led to the concentration of farside lunar maria in the Apollo-Ingenii region.

Schultz, P. H.↗

NASA NTRS2006

Spade: An H Chondrite Impact-melt Breccia that Experienced Post-shock Annealing

The low modal abundances of relict chondrules (1.8 Vol%) and of coarse (i.e. >= 2200 micron-size) isolated mafic silicate grains (1.8 Vol%) in Spade relative to mean H6 chondrites (11.4 and 9.8 vol%, respectively) show Spade to be a rock that has experienced a significant degree of melting. Various petrographic features (e.g., chromite-plagioclase assemblages, chromite veinlets, silicate darkening) indicate that melting was caused by shock. Plagioclase was melted during the shock event and flowed so that it partially to completely surrounded nearby mafic silicate grains. During crystallization, plagioclase developed igneous zoning. Low-Ca pyroxene that crystallized from the melt (or equilibrated with the melt at high temperatures) acquired relatively high amounts of CaO. Metallic Fe-Ni cooled rapidly below the Fe-Ni solws and transformed into martensite. Subsequent reheating of the rock caused transformation of martensite into abundant duplex plessite. Ambiguities exist in the shock stage assignment of Spade. The extensive silicate darkening, the occurrence of chromite-plagioclase assemblages, and the impact-melted characteristics of Spade are consistent with shock stage S6. Low shock (stage S2) is indicated by the undulose extinction and lack of planar fractures in olivine. This suggests that Spade reached a maximum prior shock level equivalent to stage S6 and then experienced post-shock annealing (probably to stage Sl). These events were followed by a less intense impact that produced the undulose extinction in the olivine, characteristic of shock stage S2. Annealing could have occurred if Spade were emplaced near impact melts beneath the crater floor or deposited in close proximity to hot debris within an ejecta blanket. Spade firmly establishes the case for post-shock annealing. This may have been a common process on ordinary chondrites (OC) asteroids.

Rubin, Alan E.↗