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At least 127 records · Page 7

Electron microscopic observations of hydrogen implantation in ilmenites

Hydrogen ion beams were found to form submicrometer, bumpy textures on the surface of ilmenite grains. From this effect, it is believed that similar bumpy textures seen on lunar ilmenite, pyroxene, and olivine grains are likely to be caused by solar wind irradiation. As a consequence, the concentration of bumpy textured grains may be a useful index of surface maturity for lunar soils. An attempt was made to search for grains with these bumpy textures in interplanetary dust and lunar and meteoritic regolith breccias in order to obtain information about the duration of their exposure to the solar wind. Solar wind irradiation was simulated on natural, terrestrial ilmenite. Hydrogen ion beams were directed at small grains and polished sections which were then examined by electron microscopy.

Blanford, G. E.↗

Significant disparity of non-basal dislocation activities in hot-rolled highly-textured Mg and Mg-3Al-1Zn alloy under tension

It is well-established that Mg-3Al-1Zn (AZ31) alloy exhibits much better tensile ductility than pure Mg. However, the underlying mechanisms for such difference still remain relatively unexplored at the dislocation level. In this work, we deformed hot-rolled highly-textured pure Mg and AZ31 samples with similar initial microstructures (i.e., grain size and texture) under tension along the rolling direction. Apparent shear banding was only observed in the pure Mg samples from the early stage of the deformation. Shear bands could act as easy paths for crack propagation, leading to low ductility in pure Mg. Apparent shear banding was not noted in deformed AZ31 samples. We then investigated the deformation mechanisms at the dislocation level using transmission electron microscopy. Systematic tilting experiments and statistical analyses of multiple grains at different strain levels revealed a significant disparity of non-basal dislocation activities between pure Mg and AZ31. For pure Mg, dislocations were activated since the early stage of plastic deformation. For AZ31, dislocations were mostly absent at all strain levels, even in the strain-to-failure samples. Non-basal dislocations, including prismatic and pyramidal dislocations, were observed. The promotion of the non-basal dislocation activities and the suppression of dislocations in AZ31 are expected to offer more sustainable hardening, which could elucidate the absence of apparent shear banding and much-improved ductility in AZ31 compared to pure Mg.

Zhao, Dexin↗

Identification of crystal plasticity model parameters by multi-objective optimization integrating microstructural evolution and mechanical data

Crystal plasticity models evolve a polycrystalline yield surface using meso-scale descriptions of deformation mechanisms. The activation of deformation mechanisms is governed by crystallography and a set of model parameters, which are typically calibrated through the fitting of mechanical data such as stress–strain curves and elastic lattice strains. Microstructural data such as phase fractions and texture evolution are used for verifying crystal plasticity parameters. In this study, we use a multi-objective genetic algorithm to identify hardening parameters from flow stress curves with an option to incorporate texture into the optimization approach. Robust, generalized objective functions are developed and used to identify sets of parameters pertaining to dislocation density-based hardening laws in visco-plastic and elasto-plastic self-consistent (VPSC and EPSC) homogenization models. First, the parameters are identified for pure Nb directly from texture using an objective function based on generalized spherical harmonics. Since texture evolution is driven by the relative contribution of active slip systems, the parameters governing the evolution of slip resistance ratios can be recovered from fitting discrete textures at a series of strains. Next, a comprehensive set of load reversal data for dual phase (DP) 780 steel is used to fit a hardening law and a back-stress law in EPSC. Finally, parameters pertaining to a complex hardening law for the evolution of slip and twinning in pure α-Ti are identified. Remarkably, using texture as an objective in combination with stress–strain objectives constrains the model of Ti to fully reproduce not only stress–strain and texture evolution but also hierarchical twinning measurements as a function of initial grain size and texture. Furthermore, given an appropriate model fit to representative experimental texture evolution, underlying twin volume fractions contributing to texture evolution can be predicted.

42 ENGINEERING↗

The impact of anisotropic thermal expansion on the isothermal annealing of polycrystalline α -uranium

Although grain growth impacts microstructural evolution in a wide variety of materials systems, the effect of anisotropic thermal expansion on grain boundary mobility and texture evolution has not been widely studied. Anisotropic thermal expansion occurs in multiple non-cubic metals, and the thermomechanical processing behavior of these materials can be better understood with further study into the impact of thermal expansion on grain boundary mobility and texture evolution. In this work, we develop a mesoscale phase field model of grain growth that includes the effect of anisotropic thermal expansion, which is applied to study polycrystalline α-uranium, a highly anisotropic metal. Three-dimensional simulations on polycrystalline a-uranium with and without thermal expansion eigenstrains are performed to study the grain boundary mobility and texture evolution as a function of temperature. A strain-free temperature of 933 K is selected, and the system is studied at within the range of 873 – 933 K at intervals of ten degrees, resulting in increasing thermal eigenstrain with decreasing temperature. We also estimate a grain boundary mobility prefactor and activation energy based on existing experimental data of isothermal annealing of α-uranium. The grain boundary mobility is found to display significant deviation from Arrhenius behavior with the inclusion of thermal expansion eigenstrain as the amount of thermal eigenstrain (and thus elastic strain energy within the system) increases. This result explains an experimentally observed grain boundary mobility deviation from Arrhenius behavior. Furthermore, the texture evolution is affected, such that the grain orientations become less random with increasing thermal eigenstrain, which could explain experimentally observed texture behavior. These results indicate that the effect of thermal expansion should be considered when predicting the thermomechanical processing behavior of α-uranium and other materials with anisotropic thermal expansion.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Experimental modeling of the cooling history of Apollo 12 olivine basalts

An analog of the Apollo 12 olivine vitrophyres has been crystallized in a 1-atm gas-mixing furnace at cooling rates ranging between 1250 and 0.7 C/hr and isothermally at degrees of supercooling ranging from 10 C to 325 C. Mineral chemistry, crystal shapes, grain sizes and textures are systematically related to cooling rate and degree of supercooling. At linear cooling rates not exceeding 40 C/hr the texture is porphyritic - large olivine crystals are set in a groundmass of finer-grained pyroxene, plagioclase, and ilmenite; a later generation of olivine never crystallizes. There are three shapes of olivine crystals in the Apollo 12 olivine vitrophyres: glomerocrysts of subhedral crystals, large subequant skeletons, and highly elongate skeletons. These result from three generations of nucleation and a two-stage cooling history - a slow preeruption stage and a rapid continuously increasing posteruption stage. It seems likely that the Apollo 12 olivine basalt magmas were erupted with olivine crystals in suspension. The nucleation temperature of olivine in cooling-rate experiments is dependent on the experimental technique, and hence results of cooling experiments should be applied with caution.

Donaldson, C. H.↗

A distinct variant of high-titanium mare basalt from the Van Serg core, Apollo 17 landing site

A fragment of basalt picked from the drive tube collected at Van Serg crater at the Apollo 17 landing site has a bulk chemistry more primitive than that of other high-titanium mare basalt groups collected at the site. The sample has a fine-grained olivine phyric, subophitic texture that is distinct from that of other high-titanium basalt samples. The grain size and texture suggest that the sample has a composition close to that of a magma. The crystallization sequence, with appearance of oxide minerals later than in other groups, and other petrographic features such as more-calcic plagioclase and early pigeonite rather than augite, are consistent with this sample representing a distinct variant of Apollo 17 high-titanium basalts. It is not related through closed-system igneous processes to any of the other mare basalt groups identified among Apollo 17 samples. Its characters emphasize the complexity of contemporaneous magma processes on the moon and the heterogeneity of that part of the mantle that was melted.

Ryder, Graham↗

Benchmarking Microscale Ductility Measurements (Final Report of the Project DE-NE0008799)

Conventional macroscale experimentation is generally considered to be straightforward with few limitations. Conversely, micro/nanoscale experimentation presents numerous challenges in loading device design, sample preparation and handling, as well as accurate understanding of grain size and local texture effects on recorded measurements. Despite these challenges, nanopillar compression, MEMs based micro-tension, and nanoindentation approaches have been able to provide fundamental contributions to the understanding of material behavior at small lengthscales. However, the overarching shortcoming of these micro/nanoscale experimentation approaches, is the inability to directly translate measurements evaluated at the nm and µm length scales (e.g., hardness) to macroscale tensile material behavior (i.e., elastic modulus, yield strength, and ductility). The objectives of the proposed study are, 1) to establish best practices for obtaining tensile microscale ductility measurements, and 2) to validate methodologies to for comparing microscale ductility measurements to macroscale ductility measurements. In order to achieve these objectives, a multi-lengthscale, multi-temperature testing protocol and simulation framework are executed first on copper as a model material to validate the following approach, and second on reactor grade Zircaloy-2. Experiments are conducted on specimens extracted from the same test piece to ensure nominally identical grain size and texture from specimens to specimen. Motivated by the need to isolate the contribution of size-effects on obtained mechanical property measurements, specimens are manufactured with thicknesses at the micro- (1-10 µm), meso- (10-100's µm), and macroscales (sub-sized ASTM E8). In-situ full-field deformation techniques (scanning electron microscopy (SEM) grid methods and optical DIC) are incorporated into testing at each specimen length-scale to capture plasticity localization and evolution. Experimental testing for all specimens is conducted at both room temperature and elevated temperatures to probe the role of thermal activation on plastic deformation accommodation processes. Simulation efforts focus on examining the mechanical behavior of microscale specimens using a finite element approach with explicitly resolved grain morphologies, and an embedded crystal plasticity model. The cost-efficient implementation method allows for the modeling of a statistically significant number of both real (i.e., digital twin) and generated microstructures to obtain an understanding of the interrelationships between specimen microstructure and geometric variables (grain size, texture, specimen geometry, etc.) on microscale mechanical behavior.

36 MATERIALS SCIENCE↗

Classification Scheme for Diverse Sedimentary and Igneous Rocks Encountered by MSL in Gale Crater

The Curiosity Rover landed in a lithologically and geochemically diverse region of Mars. We present a recommended rock classification framework based on terrestrial schemes, and adapted for the imaging and analytical capabilities of MSL as well as for rock types distinctive to Mars (e.g., high Fe sediments). After interpreting rock origin from textures, i.e., sedimentary (clastic, bedded), igneous (porphyritic, glassy), or unknown, the overall classification procedure (Fig 1) involves: (1) the characterization of rock type according to grain size and texture; (2) the assignment of geochemical modifiers according to Figs 3 and 4; and if applicable, in depth study of (3) mineralogy and (4) geologic/stratigraphic context. Sedimentary rock types are assigned by measuring grains in the best available resolution image (Table 1) and classifying according to the coarsest resolvable grains as conglomerate/breccia, (coarse, medium, or fine) sandstone, silt-stone, or mudstone. If grains are not resolvable in MAHLI images, grains in the rock are assumed to be silt sized or smaller than surface dust particles. Rocks with low color contrast contrast between grains (e.g., Dismal Lakes, sol 304) are classified according to minimum size of apparent grains from surface roughness or shadows outlining apparent grains. Igneous rocks are described as intrusive or extrusive depending on crystal size and fabric. Igneous textures may be described as granular, porphyritic, phaneritic, aphyric, or glassy depending on crystal size. Further descriptors may include terms such as vesicular or cumulate textures.

Schmidt, M. E.↗

Rocks 60618 and 65785 - Evidence for admixture of KREEP in lunar impact melts

We present evidence to support the hypothesis that the fine-grained, basaltic-textured portions of rocks 60618 and 65785 were produced by impact melting of the coarse-grained spinel-olivine anorthosite (60618) and spinel troctolite (65785) portions, coupled with admixture of approximately 33% and 63%, respectively, material of alkalic high-alumina basalt (KREEP) composition. The abundance of impact-modified rocks at the Apollo 16 site with compositional similarities to the impact melts reported here, suggests that the relations observed in these rocks are indicative of widespread impact mixing with KREEP in rocks of the lunar highlands.

Keil, K.↗

The Scattering Properties of Natural Terrestrial Snows versus Icy Satellite Surfaces

Our comparisons of the single particle scattering behavior of terrestrial snows and icy satellite regoliths to the laboratory particle scattering measurements of McGuire and Hapke demonstrate that the differences between icy satellite regoliths and their terrestrial counterparts are due to particle structures and textures. Terrestrial snow particle structures define a region in the single particle scattering function parameter space separate from the regions defined by the McGuire and Hapke artificial laboratory particles. The particle structures and textures of the grains composing icy satellites regoliths are not simple or uniform but consist of a variety of particle structure and texture types, some of which may be a combination of the particle types investigated by McGuire and Hapke.

Domingue, Deborah↗

Creep Behavior of a High-$\gamma^{\prime}$ Ni-Based Superalloy Fabricated via Electron Beam Melting

Additive manufacturing enables the fabrication of complex engineering components previously inaccessible through traditional processes. Nickel-base superalloys with large γ' volume fraction are typically considered non-weldable and therefore exhibit a propensity for cracking during the fusion process. These crack-prone materials, however, are of great importance in gas turbine engines due to their excellent high temperature creep resistance. In this study we investigate the creep behavior of IN738LC produced by the electron beam melting process. Here, we find that with appropriate post-build heat treatment the creep response of material oriented in the build direction exhibits deformation and rupture behavior comparable to that of conventionally cast IN738 & IN738LC. In the transverse direction properties fall below the expected cast behavior, however, we argue this is likely due to differences in grain scale and crystallographic texture. It may be possible to coarsen the grain morphology with appropriate process-parameter optimization in order to reduce the severity of intergranular fracture in the transverse direction. These results illustrate that high temperature properties exhibited by additively manufactured IN738LC are suitable for the hot section of gas turbine engines.

36 MATERIALS SCIENCE↗

Characterization of Al-Cu-Li Alloy 2090 Near Net Shape Extrusion

Aluminum-lithium (Al-Li) alloys near net shape extrusions are being evaluated for potential application in launch vehicle structures. The objective of this study was to determine tensile and fracture properties, corrosion resistance, and weldability of integrally stiffened panels of Al-Cu-Li alloy 2090 in the T8 temper. The microstructure was pre-dominantly unrecrystallized. Texture analyses revealed the presence of fiber components in the stiffeners and a combination of fiber and rolling components in the skin. Variations in grain morphology and texture through the extruded cross section were correlated with the tensile, fracture, and corrosion behavior. Tensile strengths at room and cryogenic temperatures of the 2090 extrusions were similar to other 2090 product forms and were higher than 2219-T87, the primary structural material in the Space Shuttle external tank; however, ductilities were lower. The fracture resistance of the 2090 extrusion was lower than 2219-T87 plate at room temperature. At cryogenic temperatures, tensile ductility and fracture behavior of the 2090 extrusion were similar to other 2090 product forms but were lower than 2219-T87 plate. The exfoliation and stress corrosion resistance of the 2090 extrusion compared favorably with the characteristics of other 2090 product forms. The weldability and weldment properties of the extrusions were similar to 2090 and 2219 plates.

Birt, M. J.↗

Crystallographic Texture, Structure, and Stress Transmission in Nugget Sandstone Examined With X‐Ray Tomography and Diffraction Microscopy

Subsurface processes in sandstones are controlled by porosity, permeability, and deformation mechanisms, all of which are controlled by a complex interplay of crystallographic rock texture, structure, and micromechanics. Texture, structure, and micromechanics have historically been studied using optical and electron microscopy of thin-sections. Here, we employed a new combination of in situ X-ray tomography and ray diffraction microscopy to study crystallographic texture, structure, and grain stresses in 3D. We examined these features in a sample of Nugget sandstone, a sandstone constituting hydrocarbon reservoirs across the American West. Our aims are threefold. First, we demonstrate the utility of X-ray diffraction microscopy probes for revealing texture, structure, and stress transmission in 3D. Second, we apply these techniques to Nugget sandstone and discuss findings in the context of prior work. Third, we study grain stress tensor evolution during mechanical compression to examine whether their heterogeneity and orientation evolution reflect that of inter-particle forces in granular materials. Our results show: (a) larger grains featured higher intra-granular misorientations, possibly from an increased prevalence of cements; (b) pores closed parallel to the loading direction and opened normal to loading; (c) grain stresses featured heterogeneity and orientations similar to inter-particle forces in non-cohesive granular materials; (d) grains featured compressive stresses in the loading direction and tensile stresses orthogonal to the loading direction, the latter resisting sample dilation and grain separation. Our work demonstrates the first known application of multi-modal X-ray tomography and diffraction microscopy to sandstone, providing new 3D insight into the nature of quartz cement and stress evolution.

high energy diffraction microscopy↗

Texture evolution as a function of scan strategy and build height in electron beam melted Ti-6Al-4V

Metal additive manufacturing (AM) enables customizable, on-demand parts, allowing for new designs and improved engineering performance. Yet, the ability to control AM metal alloy microstructures (i.e., grain morphology, crystallographic texture, and phase content) is lacking. Furthermore, this work performs corroborative neutron diffraction and large-scale electron backscatter diffraction (EBSD) measurements to assess crystallographic texture in electron beam melted (EBM) Ti-6Al-4V as a function of scan strategy and build height. Texture components for one raster and two spot melt scan strategies were evaluated using a triclinic specimen symmetry to capture all possible texture components, which were found to be considerably different than previously reported values from studies employing orthotropic specimen symmetry. This finding highlights the importance of a standard method and best practice for assessing textures produced by AM.

36 MATERIALS SCIENCE↗

Comparison of Morphologies of Apollo 17 Dust Particles with Lunar Simulant, JSC-1

Lunar dust (< 20 microns) makes up approx.20 wt.% of the lunar soil. Because of the abrasive and adhering nature of lunar soil, a detailed knowledge of the morphology (size, shape and abundance) of lunar dust is important for dust mitigation on the Moon. This represents a critical step towards the establishment of long-term human presence on the Moon (Taylor et al. 2005). Machinery design for in-situ resource utilization (ISRU) on the Moon also requires detailed information on dust morphology and general physical/chemical characteristics. Here, we report a morphological study of Apollo 17 dust sample 70051 and compare it to lunar soil stimulant, JSC-1. W e have obtained SEM images of dust grains from sample 70051 soil (Fig. 1). The dust grains imaged are composed of fragments of minerals, rocks, agglutinates and glass. Most particles consist largely of agglutinitic impact glass with their typical vesicular textures (fine bubbles). All grains show sub-angular to angular shapes, commonly with sharp edges, common for crushed glass fragments. There are mainly four textures: (1) ropey-textured pieces (typical for agglutinates), (2) angular shards, (3) blocky bits, and (4) Swiss-cheese grains. This last type with its high concentration of submicron bubbles, occurs on all scales. Submicron cracks are also present in most grains. Dust-sized grains of lunar soil simulant, JSC-1, were also studied. JSC-1 is a basaltic tuff with relatively high glass content (approx.50%; McKay et al. 1994). It was initially chosen in the early 90s to approximate the geotechnical properties of the average lunar soil (Klosky et al. 1996). JSC-1 dust grains also show angular blocky and shard textures (Fig. 2), similar to those of lunar dust. However, the JSC-1 grains lack the Swiss-cheese textured particles, as well as submicron cracks and bubbles in most grains.

Liu, Yang↗

Determination of single crystal thermal expansion in Uranium-6wt%Niobium shape memory alloy using in-situ diffraction and modeling of textured polycrystalline samples

In-situ neutron diffraction and ex-situ dilatometry experiments were performed on a chemically banded, quenched uranium-6wt% niobium shape memory alloy to study the impact of deformation-(detwinning-) induced texture on the evolution of thermally induced strains (and associated stresses). Thermal heating and cooling cycles between 5K and 473K were performed in-situ with neutron diffraction, and the lattice strain evolution is reported for the observed monoclinic α" phase. Comparisons between the measured diffraction strains and macroscopic dilatometry experiments reveal relationships between micro- and macro-level thermal expansion. Softening of the texture during heating suggests that twin boundary motion can accommodate the large internal thermal strains which are approximately 2% greater than that typically observed during the 175K heating interval used to age more randomly oriented polycrystalline material. Assuming weak constraint of neighboring grains in randomly textured polycrystals, the single crystal thermal expansion tensor is extracted from measurements of lattice strains over the range 5K to 473K. Predictions of polycrystalline thermal expansion, based upon this single crystal thermal expansion tensor, are shown to compare favorably with bulk thermal expansion observations of the as quenched microstructure. However, such a lower-bound estimate is insufficient to explain all aspects of the behavior of the textured material, where the matrix is not isotropic. In conclusion, it is hypothesized that relaxation processes which occur within the quenched microstructure during heating are responsible for the distinct thermal expansion behavior observed during the initial heating cycle compared to cooling and subsequent cycling.

36 MATERIALS SCIENCE↗

Characterization of Recrystallized Grains During Static Recrystallization of Hot-Compressed Mg–Zn–Ca Alloys Using In Situ Far-Field High-Energy Diffraction Microscopy

In this study, we explored the effect of Zn content on the static recrystallization of three 80 pct hot-compressed alloys, Mg–0.5Zn–0.1Ca wt pct (ZX050), Mg–1Zn–0.1Ca wt pct (ZX10), and Mg–3.2Zn–0.1Ca wt pct (ZX30), using far-field high-energy microscopy (ff-HEDM). Individual recrystallized grains were tracked and their 3D centroid, relative volume, and grain-averaged crystallographic orientation were measured during annealing. These measurements were used to compare the recrystallization kinetics and texture evolution of recrystallized grains in ZX alloys as a function of the Zn content. Fully recrystallized microstructures were observed for the ZX30 and the ZX10 alloys after annealing at 230 °C and 330 °C, respectively. In contrast, only a partially recrystallized microstructure for the ZX050 alloy was observed after > 1 hour of annealing at 430 °C. The resistance to recrystallization with decreasing Zn content was also confirmed by detecting faster growth rates of recrystallized grains in the ZX10 and ZX30 alloys, and slower growth rates in the ZX050 alloy. The significant recrystallization texture weakening of the ZX10 and ZX30 alloys and the development of a basal texture in the ZX05 alloy were described based on the orientation dependency of nucleation and growth of recrystallized grains. The analysis demonstrated that texture weakening was associated with increasing Zn content in Mg–Zn–Ca alloys.

Roumina, Reza [Univ. of Michigan, Ann Arbor, MI (U↗

Evaluation of Superalloy 718 Additively Manufactured Lattice Blocks

Lattice block structures made up of high temperature superalloys could offer advantages in density, efficiency, and tailored properties. Three candidate lattice designs were screened through additive manufacturing of superalloy 718. Laser powder bed fusion was applied with 718 powder to produce lattice blocks for three-dimensional octahedral unit cell designs of three heights. As-designed versus additively manufactured 718 lattices were compared, including structural dimensions, densities, defects, grain structures, crystallographic texture, and surface residual stresses. Manufactured lattice I diverged the most from its design, with both corner and center nodes merged into continuous columns. Manufactured lattice III came closest to its design, though the actual nodes and struts were still larger in cross section than in the design. Only modest grain coarsening and negligible chemical segregation were observed for all three designs, suggesting uniform thermo-physical and mechanical properties are possible. Significant tensile residual stresses were present at the surface of the manufactured blocks, with highest stresses in the building direction. Current findings indicate this concept could produce useful superalloy structures for high-temperature-capable static components requiring tailored density, and thermo-physical/mechanical properties.

super alloys↗