Micron-scale distribution controls metal(loid) release during simulated weathering of a Pennsylvanian coal shale
Abstract not provided
Singer, David M.↗
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Late-stage diagenetic concretions in the Murray formation, Gale crater, Mars
Concretions are prevalent features in the generally lacustrine deposits of the Murray formation in Gale crater. Here, we document the morphologic, textural, and chemical properties of these concretions throughout 300 m of Murray formation stratigraphy from Mars Science Laboratory observations between Sols 750–1900. We interpret these observations to constrain the timing and composition of post-depositional fluid events at Gale crater. We determine that the overall diversity of concretion morphology, size, texture, and chemistry throughout the Murray formation indicates that concretions formed in multiple, likely late diagenetic, episodes with varying fluid chemistries. Four major concretion assemblages are observed at distinct stratigraphic intervals and approximately correlate with major distinct chemical enrichments in Mg-S-Ni-Cl, Mn-P, and Ca-S, among other local enrichments. Different concretion size populations and complex relationships between concretions and veins also suggest multiple precipitation events at Gale crater. Many concretions likely formed during late diagenesis after sediment compaction and lithification, based on observations of concretions preserving primary host rock laminations without differential compaction. An upsection decrease in overall concretion size corresponds to an inferred upsection decrease in porosity and permeability, thus constraining concretion formation as postdating fluid events that produced initial cementation and porosity loss. The combined observations of late diagenetic concretions and distinct chemical enrichments related to concretions allow constraints to be placed on the chemistry of late stage fluids at Gale crater. Collectively, concretion observations from this work and previous studies of other diagenetic features (veins, alteration halos) suggest at least six post-depositional events that occurred at Gale crater after the deposition of the Murray formation.
79 ASTRONOMY AND ASTROPHYSICS↗
Predicting forming limit diagrams for magnesium alloys using crystal plasticity finite elements
The crystal plasticity finite element (CPFE) method was used to predict forming limit strains of hexagonal close-packed (HCP) polycrystalline magnesium alloy sheets, namely AZ31 and ZE10, under an isothermal temperature condition. The strain rate-dependent uniaxial tensile test data along various loading directions and an initial texture were used to determine the constitutive parameters of the crystal plasticity model. A hybrid representative volume element approach, which combines the CPFE and the Marciniak–Kuczynski model, was developed to obtain the forming limit diagram of the magnesium alloys. The predicted forming limits were in excellent agreement with the Nakazima test results. Moreover, the microscopic responses such as slip/twin activation and deformation texture changes during various loading paths from uniaxial tension to the balanced biaxial tension were comprehensively analyzed and discussed from the CPFE results to understand the underlying micro-mechanism for the macro-mechanical responses.
36 MATERIALS SCIENCE↗
Effect of amine type on acidic toxic gas adsorption at ambient conditions on modified CuBTC
We report two amine-modified copper-based Metal Organic Frameworks (MOF (CuBTC)) of different surface chemical and textural features were synthesized and used as adsorbents of acidic toxic gases (NO 2 and H 2 S) in both moist (71% relative humidity (R.H.)) and dry conditions. The initial and exhausted samples were characterized by nitrogen adsorption, powder X-ray diffraction, scanning electron microscopy, thermal gravimetric analysis and Fourier transform infrared spectroscopy. The addition of melamine prevented full growth of CuBTC crystals and resulted in amorphous-like particles with sizes less than 200 nm. The material was non-porous with a small surface area. When urea was used as an amine source, the resulting particles maintained the overall octahedral shape of the parent CuBTC MOF and the material was more porous than the parent MOF. While the urea-modified CuBTC sample performed well as an NO 2 adsorbent in the presence of moisture, the reactivity of the melamine-modified sample and its physical properties provided a favorable environment for the removal of H 2 S. The incorporation of amines into the MOF structure also resulted in surface defects /open copper sites that favored the removal of toxic gases in dry conditions. The reactivity of the adsorbents with toxic gases was demonstrated by the changes in the adsorbent colors, in texture, and in surface chemistry (organic salts, complexes, sulfides and nitrates were formed).
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
MnBi-based magnets prepared from melt-spun alloys: Effect of $α → β$ phase transformation during field annealing
The temperature of the annealing treatment applied to the MnBi alloys with the intention to stabilize the α -MnBi “low-temperature” phase – a promising material for the rare-earth-free permanent magnets – is usually kept below the range of the β -Mn 1.08 Bi “high-temperature” phase. This work is focused on the investigation of the effects of partial and complete α → β phase transformation in bulk magnetic-field-annealed magnets on their structure and magnetic properties. MnBi alloys modified with In, Mg and Sb were melt-spun, compacted to their full density and then heated in a magnetic field of 30 kOe to temperatures sufficiently high for the beginning of the α → β transformation. A heating of 15 °C/min was used which was immediately followed by cooling at the rate of 7.5 °C/min; the degree of the phase transformation was measured by in situ monitoring of changes in the sample magnetization. In all the studied alloys, the α → β transformation was found to improve the [0 0 1] fiber texture induced by the applied magnetic field, although it simultaneously decreased the coercivity. A partial transformation has resulted in a 11% increase of the maximum energy product for the Mn 50 Bi 49 Sb 0.5 In 0.5 magnet, to 8.3 MGOe, and a 3% increase for the Mn 50 Bi 46 Mg 3 Sb 0.5 In 0.5 magnet, to 12.8 MGOe. In the latter alloy, the α → β and reverse transformations were found to initially occur in well-defined pockets leading to clusters of large, highly textured α crystallites. In the Mn 50 Bi 48.5 Sb 1.5 magnet, only part of the α phase could be recovered after the transformation, which instead promoted the paramagnetic MnBi 0.9 Sb 0.1 phase.
36 MATERIALS SCIENCE↗
Spin-dependent Seebeck and Nernst effects in an ideal skyrmion gas
In this work, we theoretically and numerically study spin-dependent Seebeck and Nernst effects in 2D ferromagnetic materials with the topological spin texture (skyrmion and vortex) ideal gas. From the numerical solution of the matrix Boltzmann equation for a nonequilibrium distribution function and the Lippmann–Schwinger equation for a T-matrix we find the strong nonlinear behaviors in the thermoelectric coefficients depending on skyrmion/vortex diameters and electron concentrations. In particular, the dramatic dependences in the Seebeck and Nernst coefficients take place at larger magnetic texture sizes where the abrupt sign flip in the vortex Seebeck and Nernst coefficients occurs in the narrow region of electron concentrations. In this case the normalized Nernst coefficient changes from +5 to -7. The spin-dependent thermoelectric coefficients are proportional to T at low temperatures for all skyrmion/vortex sizes.
36 MATERIALS SCIENCE↗
Origins of high ductility exhibited by an extruded magnesium alloy Mg-1.8Zn-0.2Ca: Experiments and crystal plasticity modeling
Low ductility and strength are major bottlenecks against Mg alloys' wide applications. In this work, we systematically design the composition and fabrication process for a low-alloyed Mg-Zn-Ca alloy, showing that it can be extruded at low temperatures (~ 250 degrees C) and high speeds (~2 mm/s). After the extrusion, this alloy exhibits a substantially weakened basal texture, relatively small grain size, very high tensile elongation (~ 30%), and good strength. The origin of the considerably improved ductility was studied using a combination of three-dimensional atom probe tomography (3D-APT), transmission electron microscopy (TEM), electron backscattered diffraction (EBSD) in conjunction with surface slip trace analysis, in-situ synchrotron X-ray diffraction, and elasto-plastic self-consistent (EPSC) modeling. Co-segregation of Zn and Ca atoms at a grain boundary is observed and associated with texture weakening and grain boundary mediated plasticity, both improving the ductility. While basal slip and prismatic slip are identified as the dominant deformation systems in the alloy, the ratio between their slip resistances is substantially reduced relative to pure Mg and most other Mg alloys, significantly contributing to the improved ductility of the alloy. This Mg-Zn-Ca alloy exhibiting excellent mechanical properties and low fabrication cost is a promising candidate for industrial productions.
36 MATERIALS SCIENCE↗
Investigating microstructural evolution in SolidStir™ extruded oxide dispersion strengthened 14YWT alloy fuel cladding tube
Structural components for extreme environments require advanced materials and manufacturing processes. One such advanced material is oxide dispersion strengthened (ODS) Fe–14 wt.%Cr–3W–0.4Ti–0.3Y 2 O 3 (14YWT), which is developed for components to be used in Gen IV and fusion nuclear reactors. However, the conventional manufacturing processes to produce components, such as fuel cladding tubes, either do not retain the desired microstructural attributes or are costly and less efficient. As a result, a more attractive option is a novel manufacturing process developed on the principle of friction stir welding or processing (FSW/P) and commercially referred to as SolidStir™ Extrusion (SSE). Here this study used the SSE technique to study the manufacturing and microstructural evolution of a fuel cladding tube made of ODS 14YWT alloy. The cladding extrusion by the SSE technique involved the use of ball-milled 14YWT powders with Y, Ti, and O in the solid solution and the use of a specially designed W-25Re-Hf tool for consolidation and extrusion of the powders. A scanning electron microscope (SEM), electron backscattered diffraction (EBSD), and transmission electron microscope (TEM) were utilized for microstructural characterization. A Keyence microscope captured macrostructural photographs of the extruded tube. EBSD examination of the extruded tube on both transverse and longitudinal cross-sections showed the presence of dynamically recrystallized grains and revealed that the average grain size of the transverse cross-section was smaller than that of the longitudinal cross-section. The texture was weak and consisted of some amount of shear texture. The presence of nano-oxide clusters or precipitates of Y, Ti, and O (pyrochlores) in the extruded tube was determined by TEM. Aging heat treatment caused the average precipitate size to decrease and the density to increase compared to the as-processed condition. The results indicated that SSE is a viable tool for manufacturing fuel cladding tubes with the desired microstructural attributes.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Deformation Strengthening of Uranium and Dilute Uranium Alloys
The strength and ductility of uranium and dilute uranium alloys can be substantially improved by deformation strengthening. The yield strength of unalloyed uranium can be nearly doubled by rolling in the vicinity of 250°C. The embrittling effect of hydrogen is also overcome, eliminating the need for vacuum outgassing to obtain good ductility. Significant differences in longitudinal versus transverse tensile properties result, in part, from texture introduced by unidirectional rolling. Warm rolling of U-2.3%Nb results in both traditional strain hardening and a significant Bauschinger effect, resulting in differences between tensile and compressive yield strength. A similar combination of strain hardening and Bauschinger effect also occurs in deformation strengthened U-0.75%Ti. Warm rolling of U-0.75%Ti results in significantly better combinations of tensile yield strength and ductility than can be obtained by conventional age hardening. Warm rolling prior to aging also reduces the loss of ductility which typically accompanies conventional age hardening. Here, an approach is developed in which the effects of prior deformation on tensile and compressive yield strengths are analyzed in terms of texture, long-range dislocation, and Bauschinger effects. The Bauschinger effect is shown to vary in sign with the type of deformation, thus providing opportunities to tailor tensile and compressive properties.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
High energy X-ray characterization of the microstructure of PuGa alloy samples at macroscopic depths and non-ambient conditions
High energy (95 keV) X-rays were utilized to characterize the microstructure of eight PuGa alloy samples at room temperature and during cooling to ∼10 K. The samples had different Ga content (nominally 0-3.4 at.%), age, and history. A ninth sample, similarly characterized with neutron diffraction, was included to extend the Ga range to 7 at.%. The samples span the range from single phase α (monoclinic) to δ (face-centered cubic) PuGa, as well as a two-phase α′/δ sample. The crystallographic textures, phase fractions, lattice parameters and dislocation densities of each sample were evaluated through distinct analysis techniques. The textures of the samples were modest. In each case, the dislocation densities were relatively high, comparable to cold worked metals and metals exposed to similar radiation dose. At room temperature, the lattice parameters determined in the predominantly single-phase samples were larger than expected based on the nominal Ga concentration. The observed lattice thermal expansions of the single-phase δ samples to 10 K are self-consistent across the samples and consistent with previous measurements reported in the literature. Significantly larger thermal lattice strain is observed in the δ phase of the two-phase material due to mechanical constraint from the α′ phase, which has a three times larger thermal expansion and is much harder than the δ phase. In conclusion, the results demonstrate the unique value of high-energy X-rays for relatively routine microstructural characterization of Pu alloy samples.
36 MATERIALS SCIENCE↗
Slate – A new record for crystal preferred orientation
This report describes microstructures and preferred orientation of a Devonian slate from the Belgian Ardennes (La Fortelle quarry). The sample, composed largely of muscovite, chlorite, and quartz, displays extraordinary texture strength of muscovite, exceeding 100 multiples of random distribution (m.r.d.) for (001) pole figures and thus setting a new record for preferred orientation in rocks. Quantitative texture analysis was performed with the Rietveld method on synchrotron X-ray diffraction images. Interestingly, quartz also displays strong shape preferred orientation (SPO) as revealed by X-ray microtomography and SEM imaging but largely random crystallographic preferred orientation (CPO). In conclusion, microstructural evidence suggests that this fine-grained rock formed by recrystallization of shale under stress, with growth of phyllosilicates and dissolution and growth of quartz.
58 GEOSCIENCES↗
The partial substitution of Y with Gd on microstructures and mechanical properties of as-cast and as-extruded Mg-10Zn-6Y-0.5Zr alloy
Highlights: • The as-extruded Mg-10Zn-6Y-0.5Zr and Mg-10Zn-3Y-3Gd-0.5Zr alloys show bimodal microstructure and DRXed microstructure. • In addition to W phase, Icosahedral quasicrystal phase layer is observed at the surface of some W phase particles in as-extruded Mg-10Zn-3Y-3Gd-0.5Zr (wt. %) alloy. • The as-extruded Mg-10Zn-6Y-0.5Zr (wt. %) alloy exhibits TYS of 341 MPa, UTS of 368 MPa and elongation to failure of 6.8%. While the as-extruded Mg-10Zn-3Y-3Gd-0.5Zr (wt. %) alloy shows lower TYS of 247 MPa, UTS of 330 MPa and higher elongation to failure of 19.8%. - Abstract: Mg-10Zn-6Y-0.5Zr (wt%) alloy and Mg-10Zn-3Y-3Gd-0.5Zr (wt%) alloy with medium RE content have been fabricated by conventional casting and indirect extrusion. The as-extruded Mg-10Zn-6Y-0.5Zr (wt%) alloy shows a bimodal microstructure containing dynamic recrystallized (DRXed) grains with average grain size of 2 μm and deformed regions. In addition to the fragmented W phase particle bands distributing along the extrusion direction, large amount of nano W phase and small amount of nano β{sub 2}′ phase are precipitated in the matrix. While the as-extruded Mg-10Zn-3Y-3Gd-0.5Zr (wt%) alloy exhibits completely dynamic recrystallized microstructure with average grain size of 3 μm. The broken W phase particles are distributed homogeneously in the matrix. Icosahedral quasicrystal phase layer is observed at the surface of some W phase particles in the as-extruded Mg-10Zn-3Y-3Gd-0.5Zr alloy. The as-extruded Mg-10Zn-6Y-0.5Zr (wt%) alloy exhibits yield strength of 341 MPa, ultimate tensile strength of 368 MPa and elongation to failure of 6.8%. While the as-extruded Mg-10Zn-3Y-3Gd-0.5Zr (wt%) alloy shows lower yield strength of 247 MPa, ultimate tensile strength of 330 MPa and higher elongation to failure of 19.8%. The higher strength in the as-extruded Mg-10Zn-6Y-0.5Zr (wt%) alloy is mainly attributed to higher area fraction of unDRXed regions with strong texture and the precipitation of nano W and β{sub 2}′ phase. The fully recrystallized microstructure with weak texture and the formation of icosahedral quasicrystal phases with good coherent bond with α-Mg contribute to the good ductility of the as-extruded Mg-10Zn-3Y-3Gd-0.5Zr alloy.
36 MATERIALS SCIENCE↗
Influence of differential speed rolling ratio on the ridging behavior of ultra purified 17%Cr ferritic stainless steel
Highlights: • Differential rolling process improves ridging resistance of ferritic stainless steel. • Texture orientation inhomogeneity were attributed to non-uniform deformation. • Shear bands results in homogeneous deformation and recrystallization nucleation. • Uniform recrystallization grains and random orientation grains were obtained. - Abstract: The effect of the differential speed rolling on the ridging resistance and the crystallographic texture evolution of ultra purified 17%Cr ferritic stainless steel was investigated in order to select the optimal procedure for improving the surface quality. In the present study, the three different cold rolling processes were carried out: a conventional cold rolling and two different speed ratios asymmetric rolling. In the conventional cold rolling, the ridging of ferritic stainless steel was pronounced due to the band-like clusters of grains with similar crystallographic orientations. For differential speed rolling, ridging depth decreased and ridging was less pronounced when a higher different speed ratio was applied. The results show that severe ridging is attributed to the presence of band-like clusters of γ-fiber (<111>//ND) oriented grains. The shear bands introduced by differential speed rolling can enhance the nucleation for recrystallization both in grain interiors and grain boundaries, which can fragment the band-like clusters of similar orientation effectively, promoting the random grain orientation and improving surface quality.
36 MATERIALS SCIENCE↗
On the improvement of measurement accuracy of retained austenite in steel with X-ray diffraction
Highlights: • Improved procedure to determine austenite in steels with crystallographic texture • Extension to X-ray area detectors • Electropolishing is essential to get correct results. - Abstract: An improved measurement scheme for the determination of the retained austenite fraction with X-ray diffraction is extended to area detectors. The scheme reduces the error due to crystallographic texture in phase analysis of steel by averaging the results of diffraction patterns at different sample positions. The method is based on the standard ASTM E975, but it can be easily extended to other crystal structures, multi-phase materials or X-ray wavelengths. Phase transformation, induced by mechanical sample preparation, may lead to a significant reduction of the retained austenite fraction. Electropolishing before the measurement is beneficial to remove the layer affected by sample preparation.
36 MATERIALS SCIENCE↗
A compositional gradient Ce1−xZrxO2 buffer architecture for producing high-performance YBCO film
Highlights: • The compositional gradient CZO buffer architecture can help improve the biaxial texture of YBCO film. • The high density stacking faults are directly observed via a spherical aberration corrected transmission electron microscope. • The enhanced flux pinning force and current-carrying capacity of YBCO films are achieved as a result of lattice strains. - Abstract: In this work, YBCO films were epitaxially grown on Ce{sub 1−x}Zr{sub x}O{sub 2} (CZO) buffered yttria stabilized zirconia (YSZ) single crystal substrates through a fluorine-free sol-gel process. The influence of two different CZO buffer architectures on the microstructure and superconducting properties of YBCO films was investigated. According to XRD results in combination with (S)TEM analysis, it was confirmed that YBCO film grown on the gradient CZO buffer layer (CZO-G) exhibits better in-plane and out-of-plane texture than YBCO film deposited on the uniform CZO buffer layer (CZO-20). And besides, the superconducting performances especially the current-carrying capacity under magnetic field of the former was much higher than that of the latter, which means that the enhanced flux pinning force will be presented in YBCO film on CZO-G buffer layer. The maximum pinning force of the YBCO film grown on CZO-G buffer architecture is up to 17.67 GN/m{sup 3} @ 65 K. HR-STEM analysis shows that the stacking faults within YBCO matrix gave rise to the considerable nanoscale lattice-strains which may suppress the formation of Copper pairs and produce nanoscale non-superconducting regions served as pinning centers to significantly improve the flux pinning performance of YBCO film. Given the above, it has been implied that high-performance YBCO coated conductor can be developed by using a compositional gradient Ce{sub 1−x}Zr{sub x}O{sub 2} films as buffer architecture.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Quasi in-situ analysis of geometrically necessary dislocation density in α-fibre and γ-fibre during static recrystallization in cold-rolled low-carbon Ti-V bearing microalloyed steel
Highlights: • Average GND density is higher in gamma fibre than alpha fibre. • Higher drop in average GND density in un-recrystallized portion of gamma fibre • Fine precipitates pin the grain boundary at 700 °C 0 s. • Precipitates are coarse at 800 °C and present inside strain-free grains. - Abstract: In the present study, cold-rolled low-carbon steel is annealed at three different conditions: 700 °C for 0 s, 800 °C for 0 s and 800 °C for 2 min at the heating rate of ~10 °C/s. Recrystallization behaviour on sample surface is studied using a heated stage Scanning Electron Microscopy and Electron Backscattered Diffraction. For the lower annealing temperature of 700 °C with no dwell, almost no recrystallization is observed and microstructure resembles the as-received deformed material with the exception of occasional sub-micron sized nuclei. For the annealing conditions of 800 °C 0 s and 800 °C 2 min, onset and evolution of recrystallization is observed in-situ as a function of the initial as-cold rolled texture. Slower recovery rate of alpha fibre than gamma fibre is observed and confirmed by lower drop in average geometrically necessary dislocation (GND) density for un-recrystallized alpha fibres (1.1E+14 m{sup −2} for 700 °C 0 s, 1.4E+14 m{sup −2} for 800 °C 0 s and 4.5E+14 m{sup −2} for 800 °C 2 min) than for un-recrystallized gamma fibre grains (3.0E+14 m{sup −2} for 700 °C 0 s, 6.2E+14 m{sup −2} for 800 °C 0 s and 9.8E+14 m{sup −2} for 800 °C 2 min) during annealing. Strong gamma texture in recrystallized matrix is found for annealing conditions of 800 °C 0 s and 800 °C 2 min. From TEM characterisation it was shown that sub-grain boundaries are decorated with fine precipitates (diameter d < 15 nm) of titanium‑vanadium carbides (Ti,V)C for the annealing condition of 700 °C 0 s, which suggests that these precipitates play a major overall role in retardation of the recrystallization kinetics.
36 MATERIALS SCIENCE↗
Microstructural and micro-mechanical analysis of 14YWT nanostructured Ferritic alloy after varying thermo-mechanical processing paths into tubing
Microstructural analyses and micro-pillar compression were conducted on 14YWT nanostructured ferritic alloy (NFA) to compare different processing pathways: hydrostatic extrusion and Pilger processing with varying annealing temperatures into thin walled tubing, and after hot extrusion and cross-rolling into a plate. Hydrostatic extrusion at 815 °C resulted in the smallest grain sizes and highest yield strength of 1.20 GPa. Pilger processing with annealing at 800 °C had fine grained regions and bands of coarse grains, leading to a large variation in yield strength of 0.9–1.40 GPa. Higher annealing temperatures of 1200 °C after pilger processing significantly increased the grain size and lowered the yield strength to 1.01 GPa. These tubes showed a stronger (111) crystallographic texture in the normal direction and elongated grains in the extrusion direction. Characterization of the nano-oxides using TEM reveals more numerous, smaller oxides present in tubing processed at lower temperatures. Overall, this work shows NFA tubing after hydrostatic extrusion and pilger processing can lead to fine grained microstructures and texturing leading to higher yield strengths at lower annealing temperatures (e.g. 800 °C).
14YWT↗
Direct Observation of Tungsten Oxidation Studied by In Situ Environmental TEM
In this study, in situ environmental transmission electron microscopy (ETEM) was applied, for the first time, to investigate the thermal oxidation of a pristine and a self-ion irradiated polycrystalline tungsten, using a MEMS-based gas cell at 500 oC to 900 oC in a 1 bar 2%O2/N2 gas mixture. By tracking the dynamic evolution of the tungsten oxide scale as it initiates, grows, and sublimates during a consecutive thermal oxidation experiment, we observed two distinctive tungsten oxide microstructure – one nanocrystalline o-WO3 scale grown on W{27-1 } and W{1-1 8} and another o-WO3 scale exhibits a novel highly textured nanostructure. While the two oxide microstructures shared a similar thickness of ~200 nm after 40-minute early-stage oxidation, the nanocrystalline scale on the W{27-1 } grew much more rapidly at 800 oC than the highly textured oxide at a higher temperature of 900 oC. This suggests both the microstructure of these tungsten oxide scales as well as their oxidation kinetics are highly sensitive to the tungsten surface orientation, and such correlations also change dynamically in the course of oxidation. We also discuss the tungsten oxidation mechanism, the effects of the TEM foil thickness, and the focused ion beam (FIB) Ga+ damage on in situ ETEM oxidation.
In situ ETEM, Tungsten, Thermal oxidation, Orienta↗