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At least 109 records · Page 6

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NASA NTRS1980

Microstructure and mechanical properties of bulk and plasma-sprayed y2O3-partially stabilized zirconia

Bulk 8.0 weight percent yttria partially stabilied zirconia (PSZ) was studied by light microscopy, transmission electron microscopy, X-ray analysis, microhardness testing, and fracture toughness testing. The as received PSZ contained spheroidal and grain boundary precipitates up to 4 micrometers in size. Spheroids up to 1.26 micrometers were metastable tetragonal; large spheroids were monoclinic. Grinding the PSZ into powder did not cause a significant amount of tetragonal to transform to monoclinic. This indicates that transformation toughness is not a significant mechanism in PSZ. Aging the PSZ at 1500 C caused the fine tetragonal precipitates to grow from 0.06 to 0.12 micrometers, in 250 minutes. A peak hardness of 1400 kg/sq mm was attained after 50 minutes. Solution annealing and quenching the as received PSZ eliminated the large precipitates, but fine tetragonal precipitates reformed on quenching. Aging at 1500 C caused the fine 0.02 micrometers tetragonal precipitates to grow into plates about 0.10 by 0.50 micrometers. A peak hardness of 1517 kg/sq mm was obtained after 250 minutes. On further aging, monoclinic percipitates formed along grain boundaries. The fracture toughness of the aged and unaged solution annealed and quenched PSZ was found to be between 2 and 3 MN /square root of m cubed. This range of fracture toughness is consistent with PSZ's that do not undergo transformation toughening.

Valentine, P. G.↗

NASA NTRS1981

Microstructure and mechanical properties of bulk yttria-partially-stabilized zirconia

A commercially available bulk 4.5 mole percent yttria-Y2O3)-partially-stabilized zirconia (PSZ) was studied by light microscopy, X-ray analysis, microhardness measurement, and fracture toughness testing. The growth of the precipitates and the phase transformations were studied as a function of aging in air at 1500 C. Aging cuves were constructed for both the as-received and the solution-annealed-and-quenched materials; the curves showed hardness peaks at 1397 and 1517 kg/sq mm, respectively. A total of twelve different types of tetragonal precipitates were found. The rectangular plate-shaped tetragonal precipitates were found to have a (110) habit plane. Grinding of the Y2O3 PSZ into powder did not cause a significant amount of metastable tetragonal precipitates to transform into the monoclinic phase, thus indicating that transformation toughening is not a significant mechanism for the material. The fracture toughness of the aged and of the unaged solution-annealed-and-quenched PSZ was found to be between 2 and 3 MN/cu m/2.

Valentine, P. G.↗

NASA NTRS2021

Empirical Constraints on Progressive Shock Metamorphism of Magnetite from the Siljan Impact Structure, Sweden

Little is known about the microstructural behavior of magnetite during hypervelocity impact events, even though it is a widespread accessory mineral and important magnetic carrier in terrestrial and extraterrestrial rocks. We report systematic electron backscatter diffraction crystallographic analysis of shock features in magnetite, from a transect across the 52-km diameter ~380 Ma Siljan impact structure in Sweden. Magnetite grains in granitoid samples contain brittle fracturing, crystal-plasticity, and lamellar twins. Deformation twins along {111} with shear direction of <112> are consistent with spinel-law twins. Inferred bulk shock pressures for investigated samples, as constrained by planar deformation features (PDFs) in quartz and shock twins in zircon, range from 0–20 GPa; onset of shock-induced twinning in magnetite is observed at >5 GPa. These results highlight the utility of magnetite to record shock deformation in rocks that experience shock pressures >5 GPa, which may be useful in quartz-poor samples. Despite significant hydrothermal alteration, and variable transformation of host magnetite to hematite, shock effects are preserved, demonstrating that magnetite is a reliable mineral for preserving shock deformation over geologic time.

magnetite↗

NASA NTRS1978

The Inman, McPherson County, Kansas meteorite

The Inman meteorite (find, 1966) is a single relatively unweathered stone of 7.25 kg that contains fresh metal and only a few weathering products away from fractures. It has a pronounced chondritic texture, with 38 vol% of the meteorite being made up of chondrules of virtually all textural types. The recalculated bulk analysis, in particular ratios involving iron content, indicate that Inman is an L-group chondrite. The pronounced chondritic texture; the compositional variation of olivine, pyroxene, chromite, and ilmenite; and the presence of a fine-grained nearly opaque matrix, glass, and twinned monoclinic low-Ca pyroxene indicate that the chondrite belongs to petrologic type 3.

Keil, K.↗

DOE OSTI2021

Characterization of mechanical discontinuities based on data-driven classification of compressional-wave travel times

Wave propagation and diffusive transport phenomena are influenced by the mechanical discontinuities in material. Here this study shows that certain bulk properties of the network of low-velocity mechanical discontinuities (e.g. air-filled cracks) in a material can be characterized by processing compressional-wave travel times using traditional data-driven classification techniques. To that end, we perform three tasks in chronological order: (1) use the discrete fracture network (DFN) method to create two-dimensional (2D) numerical models of crack-bearing material embedded with various types of low-velocity mechanical discontinuities, (2) use the fast marching method (FMM) to simulate the propagation of the wave/diffusion front from a single source through the 2D crack-bearing material to multiple receivers placed on the boundary of the material, and (3) train 9 data-driven classifiers to characterize the crack-bearing materials (i.e. bulk properties of the network of mechanical discontinuities in the crack-bearing material) by learning from the simulations of travel times detected by multiple receivers placed around the crack-bearing material. The classifiers identified the orientation, spatial distribution, and dispersion of the low-velocity mechanical discontinuities. Voting classifier performs the best among the 9 classifiers. For the characterization of bulk dispersion and distribution of discontinuities, the sensors located on the adjacent boundaries are more important; whereas for the characterization of bulk orientation of discontinuities, the sensors located on the opposite side are more important.

42 ENGINEERING↗

DOE OSTI2022

Mineralogical, magnetic and geochemical data constrain the pathways and extent of weathering of mineralized sedimentary rocks

The oxidative weathering of sulfidic rock can profoundly impact watersheds through the resulting export of acidity and metals. Weathering leaves a record of mineral transformation, particularly involving minor redox-sensitive phases, that can inform the development of conceptual and quantitative models. In sulfidic sedimentary rocks, however, variations in depositional history, diagenesis and mineralization can change or overprint the distributions of these trace minerals, complicating the interpretation of weathering signatures. Here we show that a combination of bulk mineralogical and geochemical techniques, micrometer-resolution X-ray fluorescence microprobe analysis and rock magnetic measurements, applied to drill core samples and single weathered fractures, can provide data that enable the development of a geochemically consistent weathering model. This work focused on one watershed in the Upper Colorado River Basin sitting within the Mesaverde Formation, a sedimentary sandstone bedrock with disseminated sulfide minerals, including pyrite and sphalerite, that were introduced during diagenesis and subsequent magmatic-hydrothermal mineralization. Combined analytical methods revealed the pathways of iron (Fe), carbonate and silicate mineral weathering and showed how pH controls element retention or release from the actively weathering fractured sandstone. Drill core logging, whole rock X-ray diffraction, and geochemical measurements document the progression from unweathered rock at depth to weathered rock at the surface. X-ray microprobe analyses of a 1-cm size weathering profile along a fracture surface are consistent with the mobilization of Fe(II) and Fe(III) into acidic pore water from the dissolution of primary pyrite, Fe-sphalerite, chlorite, and minor siderite and pyrrhotite. These reactions are followed by the precipitation of secondary minerals such as of goethite and jarosite, a Fe-(oxyhydr)oxide and hydrous Fe(III) sulfate, respectively. Microscale analyses also helped explain the weathering reactions responsible for the mineralogical transformations observed in the top and most weathered section of the drill core. For example, dissolution of feldspar and chlorite neutralizes the acidity generated by Fe and sulfide mineral oxidation, oversaturating the solution in both Fe-oxides. The combination of X-ray spectromicroscopy and magnetic measurements show that the Fe(III) product is goethite, mainly present either as a coating on fracture surfaces in the actively weathering region of the core or more homogeneously contained within the unconsolidated regolith at the top of the core. Low-temperature magnetic data reveal the presence of ferromagnetic Fe-sulfide pyrrhotite that, although it occurs at trace concentrations, could provide a qualitative proxy for unweathered sulfide minerals because the loss of pyrrhotite is associated with the onset of oxidative weathering. Pyrrhotite loss and goethite formation are detectable through room-temperature magnetic coercivity changes, suggesting that rock magnetic measurements can determine weathering intensity in rock samples at many scales. In conclusion, this work contributes evidence that the weathering of sulfidic sedimentary rocks follows a geochemical pattern in which the abundance of sulfide minerals controls the generation of acidity and dissolved elements, and the pH-dependent mobility of these elements controls their export to the ground- and surface-water.

58 GEOSCIENCES↗

DOE OSTI2021

Thermomechanical properties and microstructures of yttrium hydride

Yttrium hydride is an optimal choice for a high-temperature moderator material in advanced thermal neutron spectrum reactors that require small core volumes. However, a complete database of the thermomechanical properties of yttrium hydride is not available yet, although it is much needed to understand and predict the moderator performance during service in reactors. In this paper, we report the properties of unirradiated bulk yttrium hydride as a function of hydrogen concentration—including density, crystal structure, specific heat capacity, thermal diffusivity, thermal conductivity, hardness, elastic/shear moduli, Poisson’s ratio, fracture strength, microstructure, and thermal stability—providing a baseline measurement for the subsequent neutron irradiation response study of yttrium hydride. Furthermore, the recommended empirical treatment of the data is suggested. In addition, other properties (i.e., hydrogen retention, thermal hydrogen migration, and irradiation response) that needs to be investigated are discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2023

In situ high-temperature 3D imaging of the damage evolution in a SiC nuclear fuel cladding material

Silicon carbide (SiC)-based nuclear fission fuel rod cladding has been considered as one of the possible designs for accident tolerant fuels. It is in the form of a SiC fibre reinforced SiC matrix composite tube (SiC f -SiC m ) with monolithic SiC outer and/or inner coating layers. This study focuses on the deformation and fracture processes in this material using in situ X-ray micro-computed tomography (XCT) at room temperature (RT) and 1200 °C in an inert gas environment in a C-ring compression loading configuration. Prior to testing, local properties and residual stresses were characterised using nanoindentation and Raman spectroscopy since they can impact the mechanical behaviour of the material. The 3D strain distribution, crack formation and propagation processes including the toughening mechanisms (e.g., crack deflection, micro-cracking, crack bridging and bifurcation) are investigated in the coating and underlying composites at RT and 1200 °C. There is no particular sequence which toughening mechanism occurs first – this is very different from the conventional toughening theory in ceramic-matrix composites under uniaxial tension loading. Indeed, no evidence of fibre pull-out or fibre fracture was observed in this SiC f -SiC m nuclear cladding material in the current C-ring compression configuration. The correlation between local measurements and bulk mechanical behaviour are discussed.

3D imaging↗

DOE OSTI2021

Handbook on the Material Properties of Yttrium Hydride for High Temperature Moderator Applications

Yttrium hydride is an optimal choice for a high-temperature moderator material in advanced thermal neutron spectrum reactors that require small core volumes. A complete database of the thermomechanical properties of yttrium hydride is not yet available, although it is much needed to understand and predict the moderator performance during service in reactors. This milestone report presents the properties of unirradiated bulk yttrium hydride as a function of hydrogen concentration—including density, crystal structure, specific heat capacity, thermal diffusivity, thermal conductivity, hardness, elastic/shear moduli, Poisson’s ratio, fracture strength, microstructure, and thermal stability. This information provides a baseline measurement for the subsequent neutron irradiation response study of yttrium hydride. The recommended empirical treatment of the data is suggested. In addition, other properties (i.e., hydrogen retention, thermal hydrogen migration, and irradiation response) requiring investigation are discussed. Also included are the Preliminary post-irradiation examination (PIE) data of yttrium hydride irradiated at 600 and 900°C to 0.1 dpa in the High Flux Isotope Reactor (HFIR). The thermophysical properties have insignificant change following this low dpa irradiation for both irradiation temperatures.

36 MATERIALS SCIENCE↗

NASA NTRS1972

Gaseous hydrogen-induced cracking of Ti-5Al-2.5Sn.

Study of the kinetics of hydrogen-induced cracking in the Ti-5Al-2.5Sn titanium alloy, which has a structure of acicular alpha platelets in a beta matrix. The crack-growth rate at low stress-intensity levels was found to be exponentially dependent on stress intensity but essentially independent of temperature. The crack-growth rate at intermediate stress-intensity levels was found to be independent of stress intensity but dependent on temperature in such a way that crack-growth rate was controlled by a thermally activated mechanism having an activation energy of 5500 cal/mole and varied as the square root of the hydrogen pressure. The crack-growth rate at stress-intensity levels very near the fracture toughness is presumed to be independent of environment. The results are interpreted to suggest that crack growth at high stress intensities is controlled by normal, bulk failure mechanisms such as void coalescence and the like. At intermediate stress-intensity levels the transport of hydrogen to some interaction site along the alpha-beta boundary is the rate-controlling mechanism. The crack-growth behavior at low stress intensities suggests that the hydrogen interacts at this site to produce a strain-induced hydride which, in turn, induces crack growth by restricting plastic flow at the crack tip.

Williams, D. P.↗

DOE OSTI2025

On the bulk compaction of brittle granular materials, part I: SeS analysis of axial compression to 4000 MPa

The bulk compaction of granular materials has been studied for decades to interpret and manage responses for soils and powder-based component fabrication, and geophysical, celestial, and ballistic impact. Their bulk or macroscopic compaction response is limited by what occurs at the granular or microstructural scale. Motivation existed to more closely examine that association specific to granular brittle materials (e.g., ceramics and glasses). That examination is offered in a series of three companion papers where Part I describes a new supplemental analysis adopted to bulk compaction response involving relatively high compaction stresses (4000 MPa). Bulk compactions of vitreous silicates and crystalline quartzes were interpreted in three ways, including that of a new analysis that considers the product of void ratio (e) and stress (S) as a function of S, hereafter referred to as “SeS analysis”. In conclusion, the SeS analysis was found to be an informative supplement to conventional bulk compaction analyses because it provides more consistent higher sensitivity for the identification of bulk density rate increase with increasing compaction (softening); a rate increase that arises from the cumulative effect of the onsets and progression of compaction-induced yielding, fracture or comminution, densification, phase change, or combinations thereof occurring at the granular or microstructural scale.

compaction↗

NASA NTRSDate not supplied

Highly Differentiated Basaltic Lavas Examined by PIXL in Jezero Crater

Textural, bulk chemical, and mineralogical data collected by PIXL(Planetary Instrument for X-ray Lithochemistry) indicate that the first rock unit (Cf-fr, Crater Floor-Fractured rough)examined by the M2020 Perseverance rover in Jezero crater is from a basaltic lava flow. This unit was originally mapped as volcanic flow[1]but has been reinterpreted as a clastic or volcaniclastic sediment[2].We here present evidence that it is a basalt flow, with implications for its petrogenesis as a highly differentiated basalt.

M E Schmidt↗

DOE OSTI2024

4D Electrical Resistivity Imaging of Stress Perturbations Induced During High–Pressure Shear Stimulation Tests

Fluid flow through fractured media is typically governed by the distribution of fracture apertures, which are in turn governed by stress. Consequently, understanding subsurface stress is critical for understanding and predicting subsurface fluid flow. Although laboratory–scale studies have established a sensitive relationship between effective stress and bulk electrical conductivity in crystalline rock, that relationship has not been extensively leveraged to monitor stress evolution at the field scale using electrical or electromagnetic geophysical monitoring approaches. In this paper we demonstrate the use time–lapse 3–dimensional (4D) electrical resistivity tomography to image perturbations in the stress field generated by pressurized borehole packers deployed during shear–stimulation attempts in a 1.25 km deep metamorphic crystalline rock formation.

58 GEOSCIENCES↗

NASA NTRS1995

The Effects of Fiber Surface Modification and Thermal Aging on Composite Toughness and Its Measurement

A detailed experimental study was conducted to establish the structure-property relationships between elevated temperature aging and fiber-matrix bonding, Mode 2 interlaminar fracture toughness, and failure modes of carbon fiber/PMR-15 composites. The fiber-matrix adhesion was varied by using carbon fibers with different surface treatments. Short beam shear tests were used to quantify the interfacial shear strength afforded by the use of the different fiber surface treatments. The results of the short beam shear tests showed that, for times up to 1000 hr, the aging process caused no changes in the bulk of the three composite materials that would degrade the shear properties of the material. Comparisons between the interlaminar shear strengths (ILSS) measured by the short beam shear tests and the GIIC test results, as measured by the ENF test, indicated that the differences in the surface treatments significantly affected the fracture properties while the effect of the aging process was probably limited to changes at the starter crack tip. The fracture properties changed due to a shift in the fracture from an interfacial failure to a failure within the matrix when the fiber was changed from AU-4 to AS-4 or AS-4G. There appears to be an effect of the fiber/matrix bonding on the thermo-oxidative stability of the composites that were tested. The low bonding afforded by the AU 1 fiber resulted in weight losses about twice those experienced by the AS 1 reinforced composites, the ones with the best TOS.

Bowles, Kenneth J.↗

NASA NTRS1987

Plates and shells containing a surface crack under general loading conditions

Various through and part-through crack problems in plates and shells are considered. The line-spring model of Rice and Levy is generalized to the skew-symmetric case to solve surface crack problems involving mixed-mode, coplanar crack growth. Compliance functions are introduced which are valid for crack depth to thickness ratios at least up to .95. This includes expressions for tension and bending as well as expressions for in-plane shear, out-of-plane shear, and twisting. Transverse shear deformation is taken into account in the plate and shell theories and this effect is shown to be important in comparing stress intensity factors obtained from the plate theory with three-dimensional solutions. Stress intensity factors for cylinders obtained by the line-spring model also compare well with three-dimensional solution. By using the line-spring approach, stress intensity factors can be obtained for the through crack and for part-through crack of any crack front shape, without recalculation integrals that take up the bulk of the computer time. Therefore, parameter studies involving crack length, crack depth, shell type, and shell curvature are made in some detail. The results will be useful in brittle fracture and in fatigue crack propagation studies. All problems considered are of the mixed boundary value type and are reducted to strongly singular integral equations which make use of the finite-part integrals of Hadamard. The equations are solved numerically in a manner that is very efficient.

Joseph, Paul F.↗

NASA NTRS1994

Strength characteristics and crack growth behavior of a composite with well aligned fibers

Continuous fiber composites have shown tremendous promise in industrial applications. Their microstructures, however, are very complex and in many instances difficult to characterize. In this project, the fracture characteristics of a specially made fiber reinforced composite with different fiber spacing are investigated. The experimental results so far have shown that after an initial transient phase the crack speed reaches a steady phase, i.e., independent of the crack length. Within the steady crack growth phase debonding along the fibers in the bridging zone grows in a self-similar manner. During the steady phase the energy dissipation per cycle is constant. Afterwards, an increase of the energy dissipation is observed that is accompanied by a decrease in crack speed. This latter trend is presumed to be the result of relatively large amounts of energy dissipated in the bulk of the specimen. Using appropriate Green's function and computer simulations, the stress intensity factor at the crack tip is evaluated for various cases of bridging stresses. In this way the effects of specimen size and fiber spacing on the overall fracture behavior of the composite system are analyzed. The steady crack speed and the steady rate of debonding have a similar power dependence on stress level. Dimensional analysis demonstrates that the particular fracture process is not governed by dimensional invariance but on the detailed micromechanisms in the bridging zone.

Botsis, John↗

NASA NTRS1997

The Effects of Fiber Surface Modification and Thermal Aging on Composite Toughness And its Measurement

A detailed experimental study was conducted to establish the structure-property relationships between elevated temperature aging and (I) fiber-matrix bonding, (2) Mode II interlaminar fracture toughness, and (3) failure modes of carbon fiber/PMR-15 composites. The fiber-matrix adhesion was varied by using carbon fibers with different surface treatments. Short beam shear tests were used to quantify the interfacial shear strength afforded by the use of the different fiber surface treatments. The results of the short beam shear tests definitely showed that, for aging times up to 1000 hr, the aging process caused no observable changes in the bulk of the three composite materials that---would degrade the shear properties of the material. Comparisons between the interlaminar shear strength (ILSS) measured by the short beam shear tests and the GII c test results, as measured by the ENF test, indicated that the differences in the surface treatments significantly affected the fracture properties while the effect of the aging process was probably limited to changes at the starter crack tip. The fracture properties changed due to a shift in the fracture from an interfacial failure to a failure within the matrix when the fiber was changed from AU-4 to AS-4 or AS-4G. There appears to be an effect of the fiber/matrix bonding on the thermo-oxidative stability of the composites that were tested. The low bonding afforded by the AU-4 fiber resulted in weight losses about twice those experienced by the AS-4 reinforced composites, the ones with the best TOS.

Bowles, Kenneth J.↗

DOE OSTI2024

Reactive flash sintering and characterization of bulk high entropy nitrides

Over the past decade, numerous high-entropy ceramics have been synthesized, often displaying attractive properties. However, the study on facile preparation of bulk high entropy nitrides (HEN) are limited, despite its broad potential applications. This research demonstrates for the first time rapid fabrication (within ∼6 min) of bulk high-entropy nitrides, especially (Al 0.17 Nb 0.17 Ta 0.17 Ti 0.32 Zr 0.17 )N, from binary nitride powder mixtures using a highly efficient reactive flash sintering (RFS) technique. X-ray diffraction (XRD) shows the HENs from RFS are near single-phase solid solutions with a rock salt crystal structure, while in situ synchrotron study carried out during RFS captured in real time the formation of HEN, which was preserved upon cooling, suggesting thermodynamic stability of the HEN phase, even up to extreme pressure (∼35.6 GPa). Microscopic analyses using SEM, STEM, and EDS reveal decent uniformity for HEN with no obvious segregation of elements, even to submicron scale. Some properties of the obtained bulk HENs are consistent with expectations. For example, their hardness and bulk modulus are close to estimates based on rule-of-mixture (ROM) values from the constituent binary nitrides. Meanwhile, some other measured properties seem to show surprises. For example, the fracture toughness for the HENs (e.g., 7.81 ± 1.40 MPa•m 1/2 or higher) turns out to be more than double of the expected ROM estimates. The significantly improved fracture toughness is attributed to the observed nano-layered structure of the HENs, despite the HEN’s cubic crystal structure and high hardness. In addition, the oxidation resistance shows improvement up till ∼800°C, possibly due to Ta doping that suppress oxygen vacancy formation in the oxide shell, while the 5-metal HEN of (Al 0.17 Nb 0.17 Ta 0.17 Ti 0.32 Zr 0.17 )N displays superconductivity (T c of ∼5–7 K from magnetism and resistivity measurements, slightly lower than ROM estimate), despite insulating property of starting AlN. Furthermore, future study combining experimental investigation using larger samples to confirm the observed increase in fracture toughness and oxidation resistance, theoretical modeling at different length scale, and more detailed structural/chemical characterization, especially at the atomic scale, are all needed to fully understand the inter-relationships between composition, processing, structure, and novel properties for these HENs and the development of related new materials for different applications.

Flash sintering↗