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At least 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
NASA NTRS2000

Advanced imaging of the macrostructure and microstructure of bone

Noninvasive and/or nondestructive techniques are capable of providing more macro- or microstructural information about bone than standard bone densitometry. Although the latter provides important information about osteoporotic fracture risk, numerous studies indicate that bone strength is only partially explained by bone mineral density. Quantitative assessment of macro- and microstructural features may improve our ability to estimate bone strength. The methods available for quantitatively assessing macrostructure include (besides conventional radiographs) quantitative computed tomography (QCT) and volumetric quantitative computed tomography (vQCT). Methods for assessing microstructure of trabecular bone noninvasively and/or nondestructively include high-resolution computed tomography (hrCT), micro-computed tomography (muCT), high-resolution magnetic resonance (hrMR), and micromagnetic resonance (muMR). vQCT, hrCT and hrMR are generally applicable in vivo; muCT and muMR are principally applicable in vitro. Although considerable progress has been made in the noninvasive and/or nondestructive imaging of the macro- and microstructure of bone, considerable challenges and dilemmas remain. From a technical perspective, the balance between spatial resolution versus sampling size, or between signal-to-noise versus radiation dose or acquisition time, needs further consideration, as do the trade-offs between the complexity and expense of equipment and the availability and accessibility of the methods. The relative merits of in vitro imaging and its ultrahigh resolution but invasiveness versus those of in vivo imaging and its modest resolution but noninvasiveness also deserve careful attention. From a clinical perspective, the challenges for bone imaging include balancing the relative advantages of simple bone densitometry against the more complex architectural features of bone or, similarly, the deeper research requirements against the broader clinical needs. The considerable potential biological differences between the peripheral appendicular skeleton and the central axial skeleton have to be addressed further. Finally, the relative merits of these sophisticated imaging techniques have to be weighed with respect to their applications as diagnostic procedures requiring high accuracy or reliability on one hand and their monitoring applications requiring high precision or reproducibility on the other. Copyright 2000 S. Karger AG, Basel.

NASA Discipline Musculoskeletal↗
NASA NTRS2005

Low Conductive Thermal Barrier Coatings Produced by Ion Beam Assisted EB-PVD with Controlled Porosity, Microstructure Refinement and Alloying Additions for High Temperature Applications

Various advanced Hafnia-based thermal barrier coatings (TBC) were applied on nickel-based superalloy coupons by electron beam physical vapor deposition. In addition, microstructural modifications to the coating material were made in an effort to reduce the thermal conductivity of the coating materials. Various processing parameters and coating system modifications were made in order to deposit the alloyed TBC with the desired microstructure and thus coating performance, some of which include applying coatings at substrate temperatures of 1150 C on both PtAl and CoNiCrAlY bond coated samples, as well as using 8YSZ as a bond layer. In addition, various characterization techniques including thermal cyclic tests, scanning electron microscopy, x-ray diffraction, thermal conductivity, and reflectivity measurements were performed. Although the coating microstructure was never fully optimized due to funding being cut short, significant reductions in thermal conductivity were accomplished through both chemistry changes (composition) and microstructural modifications.

Wolfe, Douglas E.↗
NASA NTRS2004

Effects of Initial Powder Size on the Mechanical Properties and Microstructure of As-Extruded GRCop-84

GRCop-84 was developed to meet the mechanical and thermal property requirements for advanced regeneratively cooled rocket engine main combustion chamber liners. It is a ternary Cu- Cr-Nb alloy having approximately 8 at% Cr and 4 at% Nb. The chromium and niobium constituents combine to form 14 vol% Cr2Nb, the strengthening phase. The alloy is made by producing GRCop-84 powder through gas atomization and consolidating the powder using extrusion, hot isostatic pressing (HIP) or vacuum plasma spraying (VPS). GRCop-84 has been selected by Rocketdyne, Ratt & Wlutney and Aerojet for use in their next generation of rocket engines. GRCop-84 demonstrates favorable mechanical and thermal properties at elevated temperatures. Compared to NARloy-Z, the currently used inaterial in the Space Shuttle, GRCop-84 has approximately twice the yield strength, 10-1000 times the creep life, and 1.5-2.5 times the low cycle fatigue life. The thermal expansion of GRCop-84 is 7515% less than NARloy-Z which minimizes thermally induced stresses. The thermal conductivity of the two alloys is comparable at low temperature but NARloy-Z has a 20-50 W/mK thermal conductivity advantage at typical rocket engine hot wall temperatures. GRCop-84 is also much more microstructurally stable than NARloy-Z which translates into better long term stability of mechanical properties. Previous research into metal alloys fabricated by means of powder metallurgy (PM), has demonstrated that initial powder size can affect the microstructural development and mechanical properties of such materials. Grain size, strength, ductility, size of second phases, etc., have all been shown to vary with starting powder size in PM-alloys. This work focuses on characterizing the effect of varying starting powder size on the microstructural evolution and mechanical properties of as- extruded GRCop-84. Tensile tests and constant load creep tests were performed on extrusions of four powder meshes: +140 mesh (great3er than l05 micron powder size), -140 mesh (less than or equal to 105 microns), -140 plus or minus 270 (53 - 105 microns), and - 270 mesh (less than or equal to 53 microns). Samples were tested in tension at room temperature and at 500 C (932 F). Creep tests were performed under vacuum at 500 C using a stress of 111 MPa (16.1 ksi). The fracture surfaces of selected samples from both tests were studied using a Scanning Electron Microscope (SEM). The as-extruded materials were also studied, using both optical microscopy and SEM analysis, to characterize changes within the microstructure.

Okoro, Chika L.↗
NASA NTRS2005

Mechanical Properties and Microstructure Investigation of Lead Free Solder

While the electronics industry appears to be focusing on Sn-Ag-Cu as the alloy of choice for lead free electronics assembly, ,the exact composition varies by geographic region, supplier and user. Add to that dissolved copper and silver from the printed circuit board traces and surface finish, and there can be significant variation in the final solder joint composition. A systematic study of the mechanical and microstructural properties of Sn-Ag-Cu alloys with Ag varying from 2wt% to 4wt% and Cu varying from 0.5wt% to lSwt%, was undertaken in this research study. Different sample preparation techniques (water quenched, oil quenched and water quenched followed by reflow) were explored and the resulting microstructure compared to that of a typical reflowed lead free chip scale package (CSP) solder joint. Tensile properties (modulus, 0.2% yield strength and the ultimate tensile strength) and creep behavior of selected alloy compositions (Sn-4Ag-1 X u , Sn-4Ag-OSCu, Sn- 2Ag-1 X u , Sn-2Ag-OSCu, Sn-3.5Ag-O.SCu) were determined for three conditions: as- cast; aged for 100 hours at 125OC; and aged for 250 hours at 125OC. There was no significant difference in Young's Modulus as a function of alloy composition. After an initial decrease in modulus after 100 hours at 125"C, there was an insignificant change with further aging. The distribution of 0.2% strain yield stress and ultimate tensile strength as a function of alloy composition was more significant and decreased with aging time and temperature. The microstructures of these alloys were examined using light and scanning electron microscopy (LM and SEM) respectively and SEM based energy dispersive x-ray spectroscopy (EDS). Fracture surface and cross-section analysis were performed on the specimens after creep testing. The creep testing results and the effect of high temperature aging on mechanical properties is presented for the oil quenched samples. In general the microstructure of oil quenched specimen exhibited a eutectic region of Sn with moderately dispersed Ag3Sn intermetallic, surrounded by a dendritic Sn-rich phase. The SEM images of the fracture surface indicated the presence of a tough shear surface at the initial cavity break area and a break line in the middle of specimen along the failure direction. A hyperbolic-sine creep model was adopted and used to fit the creep experiment data. The effect on the mechanical properties by adding the quaternary element bismuth to the Sn-3.5Ag-0.8Cu alloy was measured and compared with the mechanical properties of the ternary alloys. The results of this research study provide necessary data for the modeling of solder joint reliability for a range of Sn-Ag-Cu compositions and a baseline for evaluating the effects of subsequent quaternary additions.

Wang, Qing↗
NASA NTRS2006

Evolution and Control of 2219 Aluminum Microstructural Features Through Electron Beam Freeform Fabrication

The layer-additive nature of the electron beam freeform fabrication (EBF3) process results in a tortuous thermal path producing complex microstructures including: small homogeneous equiaxed grains; dendritic growth contained within larger grains; and/or pervasive dendritic formation in the interpass regions of the deposits. Several process control variables contribute to the formation of these different microstructures, including translation speed, wire feed rate, beam current and accelerating voltage. In electron beam processing, higher accelerating voltages embed the energy deeper below the surface of the substrate. Two EBF3 systems have been established at NASA Langley, one with a low-voltage (10-30kV) and the other a high-voltage (30-60 kV) electron beam gun. Aluminum alloy 2219 was processed over a range of different variables to explore the design space and correlate the resultant microstructures with the processing parameters. This report is specifically exploring the impact of accelerating voltage. Of particular interest is correlating energy to the resultant material characteristics to determine the potential of achieving microstructural control through precise management of the heat flux and cooling rates during deposition.

Taminger, Karen M.↗
NASA NTRS2006

Evolution and Control of 2219 Aluminum Microstructural Features through Electron Beam Freeform Fabrication

Electron beam freeform fabrication (EBF3) is a new layer-additive process that has been developed for near-net shape fabrication of complex structures. EBF3 uses an electron beam to create a molten pool on the surface of a substrate. Wire is fed into the molten pool and the part translated with respect to the beam to build up a 3-dimensional structure one layer at a time. Unlike many other freeform fabrication processes, the energy coupling of the electron beam is extremely well suited to processing of aluminum alloys. The layer-additive nature of the EBF3 process results in a tortuous thermal path producing complex microstructures including: small homogeneous equiaxed grains; dendritic growth contained within larger grains; and/or pervasive dendritic formation in the interpass regions of the deposits. Several process control variables contribute to the formation of these different microstructures, including translation speed, wire feed rate, beam current and accelerating voltage. In electron beam processing, higher accelerating voltages embed the energy deeper below the surface of the substrate. Two EBF3 systems have been established at NASA Langley, one with a low-voltage (10-30kV) and the other a high-voltage (30-60 kV) electron beam gun. Aluminum alloy 2219 was processed over a range of different variables to explore the design space and correlate the resultant microstructures with the processing parameters. This report is specifically exploring the impact of accelerating voltage. Of particular interest is correlating energy to the resultant material characteristics to determine the potential of achieving microstructural control through precise management of the heat flux and cooling rates during deposition.

Taminger, Karen M.↗
NASA NTRS2008

The Effects of Heat Treatment and Microstructure Variations on Disk Superalloy Properties at High Temperature

The effects of heat treatment and resulting microstructure variations on high temperature mechanical properties were assessed for a powder metallurgy disk superalloy LSHR. Blanks were consistently supersolvus solution heat treated and quenched at two cooling rates, than aged at varying temperatures and times. Tensile, creep, and dwell fatigue crack growth tests were then performed at 704 C. Gamma' precipitate microstructures were quantified. Relationships between heat treatment-microstructure, heat treatment-mechanical properties, and microstructure-mechanical properties were assessed.

Gabb, Timothy P.↗
NASA NTRS2008

Microstructure Evolution in Cut Metal Chips of Ti-6Al-4V

The microstructural evolution following metal cutting was investigated within metal chips of Ti-6Al-4V. Metal cutting was used to impose a high strain rate on the order of approx.10(exp 5)/s within the primary shear zone as the metal was removed from the workpiece. The initial microstructure of the parent material (PM) was composed of a bi-modal microstructure with coarse prior beta grains and equiaxed primary alpha located at the boundaries. After metal cutting, the microstructure of the metal chips showed coarsening of the equiaxed primary alpha grains and beta lamellar. These metallographic findings suggest that the metal chips experienced high temperatures which remained below the beta transus temperature.

Dong, L.↗
NASA NTRS2009

Microstructural Evolution of Ti-6Al-4V during High Strain Rate Conditions of Metal Cutting

The microstructural evolution following metal cutting was investigated within the metal chips of Ti-6Al-4V. Metal cutting was used to impose a high strain rate on the order of approx.10(exp 5)/s within the primary shear zone as the metal was removed from the workpiece. The initial microstructure of the parent material (PM) was composed of a bi-modal microstructure with coarse prior grains and equiaxed primary located at the boundaries. After metal cutting, the microstructure of the metal chips showed coarsening of the equiaxed primary grains and lamellar. These metallographic findings suggest that the metal chips experienced high temperatures which remained below the transus temperature.

Dong, Lei↗
NASA NTRS2010

Microstructure Modeling of 3rd Generation Disk Alloys

The objective of this program is to model, validate, and predict the precipitation microstructure evolution, using PrecipiCalc (QuesTek Innovations LLC) software, for 3rd generation Ni-based gas turbine disc superalloys during processing and service, with a set of logical and consistent experiments and characterizations. Furthermore, within this program, the originally research-oriented microstructure simulation tool will be further improved and implemented to be a useful and user-friendly engineering tool. In this report, the key accomplishment achieved during the second year (2008) of the program is summarized. The activities of this year include final selection of multicomponent thermodynamics and mobility databases, precipitate surface energy determination from nucleation experiment, multiscale comparison of predicted versus measured intragrain precipitation microstructure in quench samples showing good agreement, isothermal coarsening experiment and interaction of grain boundary and intergrain precipitates, primary microstructure of subsolvus treatment, and finally the software implementation plan for the third year of the project. In the following year, the calibrated models and simulation tools will be validated against an independently developed experimental data set, with actual disc heat treatment process conditions. Furthermore, software integration and implementation will be developed to provide material engineers valuable information in order to optimize the processing of the 3rd generation gas turbine disc alloys.

Jou, Herng-Jeng↗
NASA NTRS2010

Effect of Microstructural Parameters on the Relative Densities of Metal Foams

A detailed quantitative microstructural analyses of primarily open cell FeCrAlY and 314 stainless steel metal foams with different relative densities and pores per inch (p.p.i.) were undertaken in the present investigation to determine the effect of microstructural parameters on the relative densities of metal foams. Several elements of the microstructure, such as longitudinal and transverse cell sizes, cell areas and perimeters, ligament dimensions, cell shapes and volume fractions of closed and open cells, were measured. The cross-sections of the foam ligaments showed a large number of shrinkage cavities, and their circularity factors and average sizes were determined. The volume fractions of closed cells increased linearly with increasing relative density. In contrast, the volume fractions of the open cells and ligaments decreased with increasing relative density. The relative densities and p.p.i. were not significantly dependent on cell size, cell perimeter and ligament dimensions within the limits of experimental scatter. A phenomenological model is proposed to rationalize the present microstructural observations.

Raj, S. V.↗
NASA NTRS2012

Compositional Effects on Nickel-Base Superalloy Single Crystal Microstructures

Fourteen nickel-base superalloy single crystals containing 0 to 5 wt% chromium (Cr), 0 to 11 wt% cobalt (Co), 6 to 12 wt% molybdenum (Mo), 0 to 4 wt% rhenium (Re), and fixed amounts of aluminum (Al) and tantalum (Ta) were examined to determine the effect of bulk composition on basic microstructural parameters, including gamma' solvus, gamma' volume fraction, volume fraction of topologically close-packed (TCP) phases, phase chemistries, and gamma - gamma'. lattice mismatch. Regression models were developed to describe the influence of bulk alloy composition on the microstructural parameters and were compared to predictions by a commercially available software tool that used computational thermodynamics. Co produced the largest change in gamma' solvus over the wide compositional range used in this study, and Mo produced the largest effect on the gamma lattice parameter and the gamma - gamma' lattice mismatch over its compositional range, although Re had a very potent influence on all microstructural parameters investigated. Changing the Cr, Co, Mo, and Re contents in the bulk alloy had a significant impact on their concentrations in the gamma matrix and, to a smaller extent, in the gamma' phase. The gamma phase chemistries exhibited strong temperature dependencies that were influenced by the gamma and gamma' volume fractions. A computational thermodynamic modeling tool significantly underpredicted gamma' solvus temperatures and grossly overpredicted the amount of TCP phase at 982 C. Furthermore, the predictions by the software tool for the gamma - gamma' lattice mismatch were typically of the wrong sign and magnitude, but predictions could be improved if TCP formation was suspended within the software program. However, the statistical regression models provided excellent estimations of the microstructural parameters based on bulk alloy composition, thereby demonstrating their usefulness.

MacKay, Rebecca A.↗
NASA NTRS2014

Multiscale Analysis of Structurally-Graded Microstructures Using Molecular Dynamics, Discrete Dislocation Dynamics and Continuum Crystal Plasticity

A multiscale modeling methodology is developed for structurally-graded material microstructures. Molecular dynamic (MD) simulations are performed at the nanoscale to determine fundamental failure mechanisms and quantify material constitutive parameters. These parameters are used to calibrate material processes at the mesoscale using discrete dislocation dynamics (DD). Different grain boundary interactions with dislocations are analyzed using DD to predict grain-size dependent stress-strain behavior. These relationships are mapped into crystal plasticity (CP) parameters to develop a computationally efficient finite element-based DD/CP model for continuum-level simulations and complete the multiscale analysis by predicting the behavior of macroscopic physical specimens. The present analysis is focused on simulating the behavior of a graded microstructure in which grain sizes are on the order of nanometers in the exterior region and transition to larger, multi-micron size in the interior domain. This microstructural configuration has been shown to offer improved mechanical properties over homogeneous coarse-grained materials by increasing yield stress while maintaining ductility. Various mesoscopic polycrystal models of structurally-graded microstructures are generated, analyzed and used as a benchmark for comparison between multiscale DD/CP model and DD predictions. A final series of simulations utilize the DD/CP analysis method exclusively to study macroscopic models that cannot be analyzed by MD or DD methods alone due to the model size.

Saether, Erik↗
NASA NTRS2015

Compositional and Microstructural Evolution of Olivine During Pulsed Laser Irradiation: Insights Based on a FIB/Field-Emission TEM Study

Introduction: The use of pulsed laser irradiation to simulate the short duration, high-energy conditions characteristic of micrometeorite impacts is now an established approach in experimental space weathering studies. The laser generates both melt and vapor deposits that contain nanophase metallic Fe (npFe(sup 0)) grains with size distributions and optical properties similar to those in natural impact-generated melt and vapor deposits. There remains uncertainty, however, about how well lasers simulate the mechanical work and internal (thermal) energy partitioning that occurs in actual impacts. We are currently engaged in making a direct comparison between the products of laser irradiation and experimental/natural hypervelocity impacts. An initial step reported here is to use analytical TEM is to attain a better understanding of how the microstructure and composition of laser deposits evolve over multiple cycles of pulsed laser irradiation. Experimental Methods: We irradiated pressed-powder pellets of San Carlos olivine (Fo(sub 90)) with up to 99 rastered pulses of a GAM ArF excimer laser. The irradiated surface of the sample were characterized by SEM imaging and areas were selected for FIB cross sectioning for TEM study using an FEI Quanta dual-beam electron/focused ion beam instrument. FIB sections were characterized using a JEOL2500SE analytical field-emission scanning transmission electron microscope (FE-STEM) optimized for quantitative element mapping at less than 10 nm spatial resolutions. Results: In the SEM the 99 pulse pressed pellet sample shows a complex, inhomogeneous, distribution of laser-generated material, largely concentrated in narrow gaps and larger depressions between grains. Local concentrations of npFe0 spherules 0.1 to 1 micrometers in size are visible within these deposits in SEM back-scatter images. Fig. 1 shows bright-field STEM images of a FIB cross-section of a one of these deposits that continuously covers the top and sloping side of an olivine grain. The deposit has 3 microstructurally distinct sub-layers composed of silicate glass with varying modal fractions and size distributions of npFe( sup 0) spherules, along with nanocrystalline silicate material. A relatively thin (50-300 nm) topmost surface layer has a high-concentration of npFe0 spherules 5-20 nm in size. Element mapping shows the layer to be enriched in Fe by a factor of 2.5 relative to the olivine substrate, with Mg and Si depleted by 20% and 10% respectively. This is compositionally complementary to the underlying, middle layer of the deposit that is depleted in Fe, enriched in Mg and has a much lower npFe0 concentration. A third layer of nanocrystalline olivine occurs at the substrate interface. Discussion: The FE-STEM results suggest the topmost layer is a vapor deposit, underlain by a thicker microstructurally complex melt-generated layer. The compositional relations suggest the melt layer was partially vaporized, preferentially losing more volatile elements (e.g., Fe). The vaporized material re-condensed to form the thin, npFe(sup 0)-rich surface deposit during or immediately after the scan cycle. Nanocrystalline olivine that grew within the melt layer as it formed and cooled is similar in volume and microstructure to what we have observed in the impact melt lining of a micrometeorite impact crater in olivine. This suggest the time-temperature relations attained in the laser sample may not be too different from a micrometeorite impact. Our TEM observations, however, do not show evidence for the same level of mechanical dam-age (e.g., fracturing) seen around the natural micrometeorite crater.

Christoffersen, R.↗
NASA NTRS2018

Novel Shock Microstructures in Accessory Minerals from the Haughton Dome, Devon Island, Nunavut, Canada

The 23 km-diameter, ca. 24 Ma Haughton Dome impact structure in the Canadian Arctic on Devon Island, Nunavut (89deg41′W, 75deg22′N) occurred within a two layered target composed of a shallowly-dipping ~1700 m thick succession of Paleozoic limestones and evaporates overlying ca.1.9 Ga high grade gneisses [1, 2]. Within the structure a well preserved impact melt bearing breccia unit contains a variety of shocked clasts from the pre-impact sediments and basement gneisses [3]. Due to their high level of preservation a variety of studies have been undertaken on the clast population of the melt bearing breccia, including characterization of shock within the accessory minerals of the basement lithologies [4, 5]. This study presents high resolution electron backscatter diffraction (EBSD) microstructural data for zircon and monazite from historic samples of the basement gneiss, in which bulk shock pressures have been previously constrained based on major phases [4, 6]. Shocked zircon and monazite grains have been investigated from shock stage 1b (sample 72110), 2 (7273) and 3 (7192, Dig-9) [4, 6]. At lower shock levels zircon displays planar microstructures consistent with mechanical shock {112} twin formation [7] and deviatoric transformation to the high pressure polymorph reidite [8]. Zircon grains from shock stage three show a more chaotic microstructure with multiple orientations of tightly spaced sets of reidite that are variably recrystallized to zircon neoblasts. Monazite from lower shock stages contains a number of mechanical twin orientations that are indicative of shock deformation [9]. At higher shock pressures a lath like structure of interlocking twin orientations has been identified. This microstructure is suggestive of a reversion transformation from a high pressure polymorph [10] and is the first evidence for the transformation of monazite during shock.

Erickson, Timmons M.↗
NASA NTRS2020

Microstructure and Hardness of 57Ni –40Ti –3Hf (wt.%)

Ni-rich NiTiHf (57 wt.% Ni – 40 wt.% Ti – 3 wt.% Hf) is an intermetallic material that is superelastic, corrosion resistant and hardenable through relatively simple heat treatment procedures. The composition, microstructure and hardness of two separate lots of Ni-rich NiTiHf were investigated. The measured compositions for both lots were nominal, with total impurities in each of less than 0.01 wt%. The average grain sizes were 28.0µm and 26.4µm for the two lots. In its annealed condition (1,050°C × 48h/furnace cool to room temperature), the microstructure consisted of a B2 (cubic) NiTiHf parent phase with abundant Ni4Ti3 precipitates and a few TiC inclusions. The grain boundaries were decorated with HfO2 particles and metastable Ni3Ti2 precipitates that were cubic in structure. The average hardness varied from approximately 470HV to 490HV for the two lots. The hardened (annealed then 900°C × 2h/water quench to room temperature) microstructure consisted of a B2 NiTiHf parent phase with no precipitates, HfO2 decorating the grain boundaries and some TiC inclusions. The average hardness in this heat treatment condition was approximately 580HV for both lots. The aged (hardened then 400°C × 30min/water quench to room temperature) microstructure consisted of a B2 NiTiHf parent phase containing a high density of very fine Ni4Ti3 precipitate phase, HfO2 decorating the grain boundaries and some TiC inclusions. For each lot, the average hardness decreased slightly after aging as compared to the hardened heat treatment condition. This report is expected to serve as a reference for a forthcoming Materials Specification for the use of Ni-rich NiTiHf in flight hardware.

intermetallics, compositional analysis, Vickers ha↗
NASA NTRSDate not supplied

Deciphering Extreme Mineral Records; Microstructural Phase Heritage of Shocked Materials

High-pressure minerals such as coesite, stishovite, and reidite are often used as indicators of shock metamorphism. However, high-pressure and high-temperature phases are metastable at ambient conditions and, therefore, often revert to a more energetically favorable phase. During solid-state transformations, the crystallographic orientations of the stable polymorph are controlled by the transformation pathway from the parent. Microstructural orientation analysis using electron backscatter diffraction (EBSD) of the stable phase can reveal systematic intercrystalline orientation relationships (OR) diagnostic of solid-state transformations from these high-pressure or high-temperature polymorph phases (Cayron et al., 2006). Knowledge of polymorph stability fields for a given system can thus be used to infer minimum shock P and/or T conditions that rocks have experienced, which are otherwise unavailable using traditional thermobarometers such as element partition coefficients. Using orientation relationships to infer the former presence of mineral phases has been termed microstructural “phase heritage”, and has successfully been used to probe for evidence of extreme pressures and temperatures resulting from hypervelocity impacts. The reconstruction of polymorphs of ZrSiO4 (zircon, reidite) and ZrO2 (baddeleyite) have further elucidated the behavior of these phases under hypervelocity impact conditions (Timms et al., 2017a; White et al., 2018), and OR analysis of shocked monazite has identified a previously unrecognized tetragonal high-P polymorph (Erickson et al., 2019). Zircon will convert to the low tetragonal polymorph reidite at shock stresses above ~21 GPa. However, upon decompression at temperatures above 1200 °C reidite will revert to zircon (Kusaba et al., 1985). Recrystallized zircon neoblasts encased in impact melt often show systematic misorientation relationships of 90° about <110> indicative of reversion from the reidite (Fig. 1), and preserving cryptic evidence of the high-P history that is often erased by the post shock thermal spike (Cavosie et al., 2016). Microstructural OR analysis of a dissociated zircon corona composed of baddeleyite (monoclinic-ZrO2) has identified the former presence of cubic zirconia within impact melt glass from the Mistastin Lake impact structure, Labrador, CA. Based on stability fields in the ZrO2-SiO2 binary phase diagram, cubic zirconia records thermal conditions in excess of 2370 °C at ambient P, indicating that the Mistastin impact melt is the hottest rock identified on Earth’s surface (Timms et al., 2017b). Shock-deformed monazite (monoclinic La,Ce,ThPO4) containing lamellae comprised of interlocking laths has been identified from the Haughton Dome impact structure, Nunavut, Canada and Nördlinger-Ries Crater, southern Germany. The lath-structured lamellae are composed of four systematic orientation variants, which OR analyses indicate originate from a tetragonal parent whereby the [010]monoclinic aligns with either [100] or [010]tetragonal (Erickson et al., 2019). These results highlight utility of microstructural phase heritage analyses for the identification of unstable high-P or high-T polymorphs that uniquely record the extremely transient shock conditions produced by hypervelocity impacts.

Timmons Erickson↗
NASA NTRSDate not supplied

Toughening of Boron Carbide Composites by Hierarchical Microstructuring

Due to a unique combination of properties including high hardness, low density, chemical and thermal stability, semi-conductivity, and high neutron absorption, boron carbide (B4C) is a potential candidate for various applications involving extreme environment. However, B4C’s current application is limited because of its low fracture toughness. In this study, a hierarchical microstructure design with features including TiB2 grains and graphite platelets was used to toughen B4C by simultaneously utilizing multiple toughening mechanisms including crack deflection, bridging, and micro-crack toughening. Using field-assisted sintering technology (FAST), B4C composites with dense and hierarchical microstructure were fabricated. Previously, the fracture toughness of fabricated B4C composites was measured at micro-scale using micro-indentation to have up to 56% improvement. In this work, the B4C composites’ fracture toughness was characterized at macro-scale using four-point bending methods and compared with previous results obtained at micro-scale. Micromechanics modeling of fracture behaviors for B4C-TiB2 composites was also performed to evaluate the contributions from experimentally observed toughening mechanisms. From four-point bending tests, B4C composites reinforced with both TiB2 grains (~15 vol%) and graphite platelets (~8.7 vol%) exhibited the highest fracture toughness enhancement from 2.38 to 3.65 MPa∙m^(1/2). The measured values were lower than those obtained using micro-indentation but maintained the general trends. The discrepancy between the indentation and four-point bending test results originated from the complex deformation behaviors triggered by the high contact load during indentation tests. Through micromechanics modeling, introduced thermal residual stress due to thermal expansion mismatch between B4C and TiB2, and weak interphases at B4C-TiB2 boundaries were identified as the main causes for experimentally observed toughness enhancement. These results proved the effectiveness of hierarchical microstructure designs for B4C toughening and can provide reference for the future design of B4C composites with optimized microstructures for further fracture toughness enhancement.

composites↗