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At least 55 records · Page 3

Yield strength of CeO 2 measured from static compression in a radial diamond anvil cell

Cerium oxide (ceria, CeO 2 ) is frequently used as a standard in applications such as synchrotron and x-ray free electron lasers for calibrating x-ray wavelengths and offers the potential for understanding the high pressure properties and deformation mechanisms in a wide range of similar face centered cubic (fcc) materials. In this study, the pressure dependence of the strength of ceria was investigated up to 38 GPa using angle dispersive x-ray diffraction in a radial geometry in a diamond anvil cell. In this experiment, the difference in the stress along the axis of compression and perpendicular to the direction of compression can be determined, giving a quantity known as the differential stress. It was found that the differential stress (t), a measure of the lower bound for yield strength, initially increases rapidly from 0.35 ± 0.06 GPa to 2.2 ± 0.4 GPa at pressures of 1.8 and 3.8 GPa, respectively. Above 4 GPa, t increases more slowly to 13.8 ± 2.6 GPa at a pressure of 38 GPa. The changes in the preferred orientation (texture) of CeO 2 with pressure were also measured, allowing for the determination of active deformation mechanisms using an elasto-viscoplastic self-consistent model (EVPSC). It was found that as pressure increased, the [001] direction had a slight preferred orientation along the axis of compression. Our EVPSC model of experimental fiber (cylindrically symmetric) textures and lattice strains were most consistent with dominant slip activity along ${111}$ $\langle$$1\bar10$$\rangle$.

36 MATERIALS SCIENCE↗

Interdependence of Support Wettability - Electrodeposition Rate- Sodium Metal Anode and SEI Microstructure

Here, this study examines how current collector support chemistry (sodiophilic intermetallic Na 2 Te vs. sodiophobic baseline Cu) and electrodeposition rate affect microstructure of sodium metal and its solid electrolyte interphase (SEI). Capacity and current (6 mAh cm -2 , 0.5–3 mA cm -2 ) representative of commercially relevant mass loading in anode-free sodium metal battery (AF-SMBs) are analyzed. Synchrotron X-ray nanotomography and grazing-incidence wide-angle X-ray scattering (GIWAXS) are combined with cryogenic ion beam (cryo-FIB) microscopy. Highlighted are major differences in film morphology, internal porosity, and crystallographic preferred orientation e.g. (110) vs. (100) and (211) with support and deposition rate. Within the SEI, sodium fluoride (NaF) is more prevalent with Te-Cu versus sodium hydride (NaH) and sodium hydroxide (NaOH) with baseline Cu. Due to competitive grain growth the preferred orientation of sodium crystallites depends on film thickness. Mesoscale modeling delineates the role of SEI (ionic conductivity, morphology) on electrodeposit growth and onset of electrochemical instability.

36 MATERIALS SCIENCE↗

Crystallographic texture formation in Fe-9wt%Si alloy during deformation and phase transition at high pressure

SUMMARY The seismic anisotropy of the Earth's solid inner core has been the topic of much research. It could be explained by the crystallographic preferred orientation (CPO) developing during convection. The likely phase is hexagonal close-packed iron (hcp), alloyed with nickel and some lighter elements. Here we use high energy synchrotron X-rays to study CPO in Fe-9wt%Si, uniaxially compressed in a diamond anvil cell in radial geometry. The experiments reveal that strong preferred orientation forms in the low-pressure body-centred cubic (bcc) phase that appears to be softer than pure iron. CPO is attributed to dominant {110}<111> slip. The onset of the bcc→hcp transition occurs at a pressure of ≈15 GPa, and the alloy remains in a two phase bcc + hcp state up to 40 GPa. The hcp phase forms first with a distinct {11$\bar{2}$0} maximum perpendicular to compression. Modelling shows that this is a transformation texture, which can be described by Burgers orientation relationship with variant selection. Experimental results suggest that bcc grains oriented with <100> parallel to compression transform into hcp first. The CPO of the hcp changes only slowly during further pressure and deviatoric stress increase at ambient temperature. After heating to 1600 K, a change in the hcp CPO is observed with alignment of (0001) planes perpendicular to compression that can be interpreted as dominant (0001)<11$\bar{2}$0> slip, combined with {10$\bar{1}$2}<$\bar{1}$011> mechanical twinning, which is similar to the deformation modes suggested previously for pure hcp iron at inner core conditions.

Vasin, Roman N.↗

Emplacement of Shergottites in the Martian Crust Inferred From 3D Petrofabric and Crystal Size Distribution Analyses

Shergottites are mafic to ultramafic igneous rocks that represent a majority of known martian meteorites. They are subdivided into gabbroic, poikilitic, basaltic, and olivine-phyric categories based on differences in mineralogy and textures. Their geologic contexts are unknown so analyses of crystal sizes and preferred orientations have commonly been used to infer where shergottites solidified. Such environments range from subsurface cumulates to shallow intrusives to extrusive lava flows, which all have contrasting implications for interactions with crustal material, cooling histories, and potential in situ exposure at the surface. In this study, we present a novel three-dimensional (3D) approach to better understand the solidification environments of these samples and improve our knowledge of shergottites’ geologic contexts. Shape preferred orientations of most phases and crystal size distributions of late-forming minerals were measured in 3D using X-ray computed tomography (CT) on eight shergottites representing the gabbroic, poikilitic, basaltic, and olivine-phyric categories. Our analyses show that highly anisotropic, rod-like pyroxene crystals are strongly foliated in the gabbroic samples but have a weaker foliation and a mild lineation in the basaltic sample, indicating a directional flow component in the latter. Star volume distribution analyses revealed that most phases (maskelynite, pyroxene, olivine, and oxides/sulfides) preserve a foliated texture with variable strengths, and that the phases within individual samples are strongly to moderately aligned with respect to one another. In combination with relative cooling rates during the final stages of crystallization determined from interstitial oxide/sulfide crystal size distribution analyses, these results indicate that the olivine-phyric samples were emplaced as shallow intrusives (e.g., dikes/sills) and that the gabbroic, poikilitic, and basaltic samples were emplaced in deeper subsurface environments.

Martian meteorites↗

Strain Measurements of Chondrules and Refraction Inclusion in Allende

This study uses traditional strain measurement techniques, combined with X-ray computerized tomography (CT), to evaluate petrographic evidence in the Allende CV3 chondrite for preferred orientation and to measure strain in three dimensions. The existence of petrofabrics and lineations was first observed in carbonaceous meteorites in the 1960's. Yet, fifty years later only a few studies have reported that meteorites record such features. Impacts are often cited as the mechanism for this feature, although plastic deformation from overburden and nebular imbrication have also been proposed. Previous work conducted on the Leoville CV3 and the Parnallee LL3 chondrites, exhibited a minimum uniaxial shortening of 33% and 21%, respectively. Petrofabrics in Allende CV3 have been looked at before; previous workers using Electron Back Scatter Diffraction (EBSD) found a major-axis alignment of olivine inside dark inclusions and an "augen"-like preferred orientation of olivine grains around more competent chondrules

Tait, Alastair W.↗

Significant enhancement of magnetocaloric effect in a NiMnCuGa Heusler alloy through textural modification

Magnetocaloric materials are of increasing interest to bring magnetic refrigeration to everyday households and drastically impact the energy demands for temperature control devices. In this work, a polycrystalline Heusler alloy of composition Ni2Mn0.76Cu0.24Ga with coinciding structural and magnetic transformation temperatures was subjected to compressive stress assisted thermal cycling (SATC) to enhance the magnetic properties by inducing a preferred orientation in the martensite. Isofield magnetization measurements showed a sharpening of the transformation between ferromagnetic martensite and paramagnetic austenite due to SATC. In isothermal magnetization measurements, SATC was seen to increase the magnetostructural coupling. With a 2 T applied magnetic field, the magnetocaloric effect (MCE) increased from ∼10 to ∼25 J/kg K and the refrigeration capacity (RC) almost doubled due to SATC. Heat capacity measurements were largely unaffected by SATC. The change in adiabatic temperature was estimated by using Cp and change in magnetic entropy (ΔSM) calculations. SATC was seen to increase ΔTad from ∼1.2 K to 2 K for an applied magnetic field of 2 T. Neutron diffraction measurements revealed highly textured martensite in the as received state that rotated to a more ideal preferred orientation after SATC that enhanced the magnetostructural transformation; and thus, improving the MCE and ΔTad.

McLeod, M. V. (ORCID:0000000329883516)↗

Stream pattern analysis using optical processing of ERTS imagery of Kansas

A spatial frequency analysis was carried out to obtain large-scale geologic and other ground pattern spatial frequency and orientational data from an optical data processing system using Earth Resources Technology Satellite-1 (ERTS-1) imagery of Kansas as input. The Diffraction Pattern Sampling Unit (DPSU) of the optical data processing system consists of a photodiode array containing 32 wedge-shaped photodiodes and 32 annular ring diodes. The curve obtained from the intensity distribution of the frequency spectrum yielded by the ring diodes gives the spatial frequency contributions due to ground features on the image. The curve obtained from the wedge-shaped diodes indicates the orientation of features in the sample area. Ten sample sites were used for each of eight geologic-physiographic regions. Comparison of ERTS-1 images with their respective spatial frequency and orientational curves reveals that preferred orientations of drainage produce recognizable peaks.

Mccauley, J.↗

Fatigue damage study in aluminum-2024 T3 alloys

The grain structure of aluminum 2024, a commonly used commercial alloy is investigated, and these findings are correlated with the fatigue property of the material. Samples of aluminum 2024 were polished and etched in different reagents. Optical micrographs (at 500X) of samples etched in Keller's reagent revealed grain boundaries as well as some particles present in the microstructure. Normal x-ray scans of samples etched for different intervals of time in Keller's reagent indicate no significant variations in diffraction peak positions; however, the width of the rocking curve increased with the time of etching. These results are consistent with the direct dependence of the width of the rocking curve on the range of grain orientation. Etching removes the preferred orientation layer of the sample produced by polishing; thereby, causing the width to increase.

Ferguson, Milton W.↗

Display and lighting devices comprising phosphorescent excimers with preferred molecular orientation as monochromatic emitters

An organic light emitting diode having a substrate, a first electrode, a hole transporting layer proximate the first electrode, a second electrode, an electron transporting layer proximate the second electrode, and an emissive layer between the hole transporting layer and the electron transporting layer. The emissive layer includes a square planar tetradentate platinum or palladium complex, and excimers formed by two or more of the complexes are aligned such that emitting dipoles of the excimers are substantially parallel to a surface of the substrate.

Li, Jian↗

Preferred Secondary Crystal Orientation For Turbine Blades

Directional solidification of single-crystal turbine blades, so secondary and primary, crystallographic orientation occurs on preferred axis, greatly increases resistance to fatigue. Technique lengthens lives of parts and reduces variation in longevity among parts.

Fritzemeier, Leslie G.↗

Uniaxial stress increases layer stacking disorder in calcium silicate hydrates with low calcium content

The long-term stress response of concrete is controlled by the intergrain and intragrain interactions of calcium-silicate-hydrates (C-S-H), nanocrystalline forms of tobermorites. To investigate both types of interactions, we examined the deviatoric stress response of 11 Å tobermorite powder with X-ray diffraction, finding that its layer stacking (i.e., sliding) disorder significantly increases. A similar experiment was performed on nanocrystalline C-S-H powders before and after applying a 360 MPa uniaxial stress. Layer stacking disorder (in the form of intragrain deformation) increases when there is low water content and when the basal spacing is large. We also find that grains with a smaller thickness-to-diameter aspect ratio are first to develop preferred orientation (in the form of intergrain sliding), facilitated by gel water. Furthermore, these findings show that intragrain deformations in C-S-H can occur at relatively low stresses and provide insights into the creep mechanism of C-S-H.

36 MATERIALS SCIENCE↗

Deformation of Hydrous Phases Egg [AlSiO 3 (OH)], δ [AlO(OH)] and Stishovite [Si 1‐n H 4n O 2 ] Relevant to Anisotropy of the Earth's Mantle

Seismic anisotropy of the Earth's mantle has been mostly attributed to crystallographic preferred orientation (CPO) generated during subduction and convection of an anhydrous mantle. But some hydrous phases are also stable at mantle conditions. Here we present results from diamond-anvil cell deformation experiments at high pressure and temperature on hydrous phases Egg [AlSiO 3 (OH)], δ [AlO(OH)] and hydrous stishovite [Si 1-n H 4n O 2 ], transformed from the clay mineral kaolinite. They develop strong CPO during axial compression, suggesting that they likely contribute to seismic anisotropy and heterogeneity in the mantle. Comparing experimental results with viscoplastic polycrystal plasticity models suggest that phase Egg deforms dominantly by (001) slip, δ by (010) slip and stishovite by {100} slip which could be incorporated in future models of mantle geodynamics.

58 GEOSCIENCES↗

Exploring microstructures and anisotropies of serpentinites

Serpentine minerals have received a lot of attention because of their unique crystal structures, their wide occurrence in orogenic belts and their potential role in contributing seismic anisotropy in subducting slabs. Several studies have investigated crystal preferred orientation (CPO) in high temperature antigorite serpentinites from Japan, the Alps, Spain, Cuba and Tibet, documenting significant crystal alignment. However, only a limited number of lower grade serpentines have been explored to date. Mainly because of submicroscopic microstructural heterogeneities CPO cannot be measured with conventional methods such as optical microscopy and EBSD. In this study 15 serpentinites from different tectonic settings in California, the Central Alps and Northern Spain have been investigated, mainly with high energy synchrotron X-ray diffraction, to quantify bulk crystal alignment. We find that CPO is strong on sheared surfaces of fractured blocks and secondary veins but the bulk of most serpentinite samples, except high-grade recrystallized antigorite serpentinite, show only weak crystal alignment. Correspondingly calculated seismic anisotropy based on CPO is not very significant. This is supported by very heterogeneous microstructures as documented with SEM and TEM analyses.

58 GEOSCIENCES↗

In situ deformation of antigorite-olivine two-phase mixtures: Implications for dynamics and seismic anisotropy in the mantle wedge

Water released from hydrous minerals in subducting slabs reacts with the overlying plate, resulting in widespread serpentinization in the mantle wedge. Deformation of serpentinized peridotites has been invoked to explain forearc seismic anisotropy, yet studies of the mechanical properties and deformation behaviors of serpentine-bearing multiphase aggregates remain limited. Here we deformed olivine-antigorite mixtures containing 70, 50, and 20 vol.% of antigorite at 2.5 – 7.6 GPa, 673 K and strain rates of ∼10 –5 –10 –4 s –1 . Elasto-viscoplastic self-consistent simulations, constrained by synchrotron X-ray diffraction (XRD) data, were used to estimate lattice strain, stress–strain partitioning, crystallographic preferred orientations (CPO) development, and aggregate strength. Selected run products were also analyzed by electron backscatter diffraction for comparison with the CPO results obtained from XRD experiments. We found olivine transitions from A- or B-type to C-type when antigorite fraction drops to 20 vol.%, coinciding with a microstructural change from interconnected weak layers to a load-bearing framework (LBF). An additional run on a sample Atg50/Ol50 with preexisting microstructures suggested the formation of LBF was promoted by these microstructures, although the preexisting antigorite CPO has been overprinted at 20.8 % strain and could be erased completely by subsequent deformation in nature. Estimated viscosity of the two-phase mixtures suggests that low-degree serpentinization (≤20 %) in the mantle wedge may increase the strength of olivine-rich peridotite and hinder slab-mantle decoupling, whereas high-degree serpentinization (≥50–70 %) weakens the peridotite and favors decoupling if sufficient viscosity contrast (>10) develops. Seismic anisotropy shows a nonlinear dependence on antigorite fraction: antigorite CPO governs the anisotropy of the mixtures with ≥50 vol.% antigorite, whereas olivine CPO dominates at low fractions (∼20 vol.%). The presence of pre-existing microstructures reduces seismic anisotropy of the deformed mixtures, however the persistence of pre-existing CPO in actively subducting slabs remains uncertain, making their significance over geological timescales questionable.

Crystallographic preferred orientation↗

Microstructure and CPO evolution of dynamically recrystallized olivine during complex deformation conditions: a full-field numerical modeling approach

The rheological properties of mantle rocks are strongly dependent on their crystallographic preferred orientation (CPO). Olivine CPO, defined by the orientation of seismically fast [100] axes parallel to flow direction, is also thought to be a dominant contributor to seismic anisotropy in the Earth's upper mantle. However, the amount of deformation needed to overprint a new CPO on a pre-existing fabric and the impact of the inherited CPOs on the transient microstructure evolution, remain unknown. This study employs a full-field numerical approach (VPFFT-ELLE) to explore the dynamic recrystallization and microstructural evolution of olivine polycrystalline aggregates under complex deformation conditions. We test four combinations of successive pure shear and simple shear boundary conditions. Findings indicate that inherited CPOs influence subsequent deformation in a manner dependent on the kinematic relationship between successive stages. In all cases, a minor strain increment (ε ∼0.3–0.6) is sufficient to erase the previous microstructure and CPO. However, when deformation conditions change dramatically (e.g., stretching direction changes orthogonally), the intensity of the new CPO developed is significantly lower and strain distribution are specially altered. During a transient strain stage, pre-existing microstructures undergo extensive reworking, especially when deformation conditions are changed dramatically, such as switching from simple shear to a pure shear condition with a parallel shortening direction relative to the stretching direction. We estimate the significance of these results in interpreting observations of seismic velocity anisotropy, concluding that P-wave seismic anisotropy is significantly and positively correlated with the evolution of olivine CPO with deformation history. This research underscores the transient nature of microstructural rearrangement in olivine aggregates and the necessity for caution in interpreting seismic anisotropy in regions with complex deformation histories, as inherited CPOs can influence current fabric development and induce deviation to the present deformation conditions.

36 MATERIALS SCIENCE↗

In Situ Analysis of Martian Phyllosilicates Using the Chemin Minerological Instrument on Mars Science Laboratory

The CheMin minerological instrument on Mars Science Laboratory (MSL'09) [1] will return quantitive Xray diffraction data (XRD) and quantative X-ray fluorescence data (XRF;14<Z<92) from scooped soil samples and drilled rock powders collected from the Mars surface. Samples of 45-65 mm 3 from material sieved to less than 150 micrometers will be delivered through a funnel to one of 27 reusable sample cells (five additional cells on the sample wheel contain diffraction of fluorescence standards). Sample cells are 8-mm diamater discs with 7-micrometer thick Mylar or Kapton windows spaced 170 micrometers apart. Within this volume, the sample is shaken by piezoelectric vibration at sonic frequencies, causing the powder to flow past a narrow, collimated -ray beam in random orientation can be obtained even from minnerals exhibiting strong preferred orientation such as phylosilicates.

Blake, David F.↗