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At least 1,153 records · Page 64

Czochralski growth and characterization of the multicomponent garnet (Lu 1/4 Yb 1/4 Y 1/4 Gd 1/4 ) 3 Al 5 O 12

This work demonstrates the potential for practical scalable growth of complex garnets and evaluates the implications of a multicomponent composition in the optical quality and elemental distribution of a Czochralski-grown crystal. Furthermore, our experimental approach was designed to elucidate the relation between a complex garnet composition ( Lu 1 / 4 Yb 1 / 4 Y 1 / 4 Gd 1 / 4 ) 3 Al 5 O 12 , crystal growth parameters, crystal structural, and elemental homogeneity. Our hypothesis is that combining multiple rare earths (REs) that will fractionally occupy the dodecahedral site in the aluminum garnet structure will result in a stable, single garnet compound that can be grown by the Czochralski method. Single-crystal and powder x-ray diffraction indicated a single garnet phase with an increasing unit cell volume from seed to tail. In addition, we propose that the pattern of elemental segregation will be based on the deviation of the ionic radius of each constituent RE from the average RE ionic radius of the multicomponent garnet. Electron probe microanalysis revealed that ions that are smaller than that average ( Lu 3 + and Yb 3 + ) are preferentially incorporated in the crystal, while elements that are larger than that average ( Gd 3 + ) are rejected. The ionic radius of Y 3 + is close to that average and yttrium segregation was minimal. The concentrations of the four REs are closer to stoichiometric on the tail end of the boule. Scanning electron microscopy and energy-dispersive x-ray spectroscopy analysis reveal Gd-rich inclusions with eutectic microstructures in the tail end of the boule.

36 MATERIALS SCIENCE↗

Pinning Characteristics of Zr and Hf- Added REBCO Coated Conductors Made by Advanced MOCVD in Low-to-High Magnetic Fields

BaMO 3 (M=Zr, Hf) pinning centers introduced in REBa 2 Cu 3 O 7-x (REBCO and RE = rare earth) coated conductors yield superior performance in high magnetic fields. We present the critical current density J c over a temperature range of 4.2-77 K and magnetic fields of 0-14 T (B || c-axis), of 5-15 mol.% Zr- and Hf-added REBCO 4+ μm thick film tapes fabricated by advanced metal organic chemical vapor deposition (A-MOCVD). The morphology of self-assembled BMO nanorods aligned along c-axis is found to be dependent on the Zr/Hf content. We also observe a correlation between the density of RE 2 O 3 in-plane nano-precipitates and the continuity and concentration of BMO nanorods in films of different Ba content. It is found that the (Ba+M)/Cu (M=Zr, Hf) content in REBa 2 Cu 3 O 7-x affects the shape of pinning force density curves over a wide magnetic field range and temperatures below 20 K. Another remarkable observation is the similarity in the critical current properties of Hf and Zr -added REBCO films as function of (Ba+M)/Cu content at intermediate to high range of (Ba+M)/Cu content. As a result, a quantitative analysis of pinning efficiency and correlation with the microstructure of Zr and Hf- added REBCO coated conductors is discussed.

2G high-temperature superconductor (2G-HTS)↗

Quantification and Uncertainty in Particle Morphological Analysis

A key part of forensic analysis of interdicted nuclear materials is examining the microstructure of the materials, which are frequently in the form of particulates. We are developing methods for quantifying the morphology of particle sets imaged using scanning electron microscopy. In order to use this data effectively, we need to understand the uncertainties involved in measuring the morphology of particles. This presentation discusses the sources of uncertainty in scanning electron microscopy, and presents the results of an internal user test of the MAMA software package being developed under a DHS Transformational and Applied Research program. The steps required to establish morphological standards similar to NIST standards are discussed.

36 MATERIALS SCIENCE↗

Creep and Rupture Strength of an Advanced CVD SiC Fiber

In the as-produced condition the room temperature strength (approx. 6 GPa) of Textron Specialty Materials' 50 microns CVD SiC fiber represents the highest value thus far obtained for commercially produced polycrystalline SiC fibers. To understand whether this strength can be maintained after composite processing conditions, high temperature studies were performed on the effects of time, stress, and environment on 1400 deg. C tensile creep strain and stress rupture on as-produced, chemically vapor deposited SiC fibers. Creep strain results were consistent, allowing an evaluation of time and stress effects. Test environment had no influence on creep strain but I hour annealing at 1600 deg. C in argon gas significantly reduced the total creep strain and increased the stress dependence. This is attributed to changes in the free carbon morphology and its distribution within the CVD SiC fiber. For the as-produced and annealed fibers, strength at 1400 deg. C was found to decrease from a fast fracture value of 2 GPa to a 100-hr rupture strength value of 0. 8 GPa. In addition a loss of fast fracture strength from 6 GPa is attributed to thermally induced changes in the outer carbon coating and microstructure. Scatter in rupture times made a definitive analysis of environmental and annealing effects on creep strength difficult.

Goldsby, J. C.↗

Effects of Long Term Thermal Exposure on Chemically Pure (CP) Titanium Grade 2 Room Temperature Tensile Properties and Microstructure

Room temperature tensile testing of Chemically Pure (CP) Titanium Grade 2 was conducted for as-received commercially produced sheet and following thermal exposure at 550 and 650 K for times up to 5,000 h. No significant changes in microstructure or failure mechanism were observed. A statistical analysis of the data was performed. Small statistical differences were found, but all properties were well above minimum values for CP Ti Grade 2 as defined by ASTM standards and likely would fall within normal variation of the material.

Ellis, David L.↗

Unit-Sphere Multiaxial Stochastic-Strength Model Applied to Anisotropic and Composite Materials

Models that predict the failure probability of brittle materials under multiaxial loading have been developed by authors such as Batdorf, Evans, and Matsuo. These "unit-sphere" models assume that the strength-controlling flaws are randomly oriented, noninteracting planar microcracks of specified geometry but of variable size. This methodology has been extended to predict the multiaxial strength response of transversely isotropic brittle materials, including polymer matrix composites (PMCs), by considering (1) flaw-orientation anisotropy, whereby a preexisting microcrack has a higher likelihood of being oriented in one direction over another direction, and (2) critical strength, or K (sub Ic) orientation anisotropy, whereby the level of critical strength or fracture toughness for mode I crack propagation, K (sub Ic), changes with regard to the orientation of the microstructure. In this report, results from finite element analysis of a fiber-reinforced-matrix unit cell were used with the unit-sphere model to predict the biaxial strength response of a unidirectional PMC previously reported from the World-Wide Failure Exercise. Results for nuclear-grade graphite materials under biaxial loading are also shown for comparison. This effort was successful in predicting the multiaxial strength response for the chosen problems. Findings regarding stress-state interactions and failure modes also are provided.

Nemeth, Noel, N.↗

Carbon-bearing fluids at nanoscale interfaces

The behaviour of fluids at mineral surfaces or in confined geometries (pores, fractures) typically differs from their bulk behaviour in many ways due to the effects of large internal surfaces and geometrical confinement. We summarize research performed on C-O-H fluids at nanoscale interfaces in materials of interest to the earth and material sciences (e.g., silica, alumina, zeolites, clays, rocks, etc.), emphasizing those techniques that assess microstructural modification and/or dynamical behaviour such as gravimetric analysis, small-angle (SANS) neutron scattering, and nuclear magnetic resonance (NMR). Molecular dynamics (MD) simulations will be described that provide atomistic characterization of interfacial and confined fluid behaviour as well as aid in the interpretation of the neutron scattering results.

geofluids↗

Irradiation Testing of Additively Manufactured Materials for LWR Applications: Alloy 718 and 316L Stainless Steel

The objective of this NSUF Project is to assess the changes in irradiated additively manufactured (AM) material properties as compared to non-irradiated material. Type 316L stainless steel and Alloy 718 samples were produced using Direct Metal Laser Melting (DMLM) fabrication. Materials produced from this fabrication method have several potential applications within the nuclear industry as reactor internal repair parts, fuel debris resistant filters, or fuel spacers within existing light water reactors (LWRs). AM materials have been shown to achieve equivalent mechanical behavior in simulated reactor environments as compared to wrought materials, but have significantly more flexibility when it comes to unique design features. The increased component design flexibility makes these AM materials an attractive choice for both current LWR applications as well as for small modular reactor (SMR) designs. Prior to use of these materials in reactor fleet operation, the industry as a whole must evaluate the effects of irradiation on their material properties. Standard 0.4 inch thick Compact Tension specimens and SSJ3 type tensile bars were neutron irradiated at the Advanced Test Reactor to ~1 dpa for the purpose of performing a variety of mechanical tests in a range of simulated environments applicable to LWRs. For the ductile austenitic Type 316L stainless steel, the irradiated data will be used to confirm that the AM process produces materials with properties that are equivalent to wrought materials under testing conditions applicable to LWR operation. Transmission electron microscopy analysis was also performed in order to understand microstructural and microchemical changes induced in each material in response to neutron irradiation. If possible, data collected from these AM 316L samples will be used to remove fluence limits from specifications of ASME code cases for this alloy, which will give vendors much more flexibility in building future components.

36 - MATERIALS SCIENCE↗

Ground state microstructure of a ferrofluid thin layer

Using a fine weave of theoretical analysis and computer simulations, we found various aggregates of magnetic single-domain nanoparticles, which can form in a quasi-two-dimensional (q2D) ferrofluid layer at low temperatures. Our theoretical investigation allowed us to obtain exact expressions and their asymptotes for the energies of each configuration. Thus, for ferrofluid q2D layers it proved possible to identify the ground states as a function of the particle number, size, and other system parameters. Our suggested approach can be used for the investigation of ground state structures in systems with more complex interparticle interactions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Optimizing Discharge Capacity of Li-O 2 Batteries by Design of Air-Electrode Porous Structure: Multifidelity Modeling and Optimization

We develop a new mathematical framework to study the optimal design of air electrode microstructures for lithium-oxygen (Li-O2) batteries. It can eectively reduce the number of expensive experiments for testing dierent air-electrodes, thereby minimizing the cost in the design of Li-O2 batteries. The design parameters to characterize an air-electrode microstructure include the porosity, surface-to-volume ratio, and parameters associated with the pore-size distribution. A surrogate model (also known as response surface) for discharge capacity is rst constructed as a function of these design parameters. The surrogate model is accurate and easy to evaluate such that an optimization can be performed based on it. In particular, a Gaussian process regression method, co-kriging, is employed due to its accuracy and eciency in predicting high-dimensional responses from a combination of multidelity data. Specically, a small amount of data from high-delity simulations are combined with a large number of data obtained from computationally ecient low-delity simulations. The high-delity simulation is based on a multiscale modeling approach that couples the microscale (pore-scale) and macroscale (device-scale) models. Whereas, the low-delity simulation is based on an empirical macroscale model. The constructed response surface provides quantitative understanding and prediction about how air electrode microstructures aect the discharge performance of Li-O2 batteries. The succeeding sensitivity analysis via Sobol indices and optimization via genetic algorithm ultimately oer a reliable guidance on the optimal design of air electrode microstructures. The proposed mathematical framework can be generalized to investigate other new energy storage techniques and materials.

25 ENERGY STORAGE↗

The effect of milling time on the synthesis of Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy

In the present work, nanocrystalline Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy was produced by mechanical alloying from mixtures of pure crystalline Cu, Mg, Ti and Ni powders using a Fritsch planetary ball mill with a ball to powder ratio of 10:1. Morphological changes, microstructural evolution and thermal behaviour of the Cu-Mg-Ti-Ni powders at different stages of milling were characterised by X-ray diffraction (XRD), scanning electron microscopy with energy-dispersive X-ray detection (SEM/EDX) and differential thermal analysis (DTA). This alloy resulted in formation of single phase solid solution with FCC structure α-Cu (Mg, Ti, Ni) after 80 h of milling. In the initial stage of milling different sized and shaped elemental powders became uniform during mechanical alloying. The homogeneity of the Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy increased with increasing milling time. The EDX result also confirmed the compositional homogeneity of the powder alloy. The crystallite size of alloy was calculated below 10 nm from XRD data.

36 MATERIALS SCIENCE↗

A critical review of the history of fabricating monolithic U-Mo fuel plates

The fabrication of monolithic uranium-molybdenum alloy fuels, specifically those developed for high-performance research and test reactors, began in the early 2000s. The primary fuel form consists of uranium alloyed with 10-wt% molybdenum in a thin foil coated with zirconium and encapsulated in aluminum-6061 cladding. Over the years, the process has evolved with different types of casting, heat treatments, rolling schedules, and cladding applications. This review examines the history of these fabrication processes and their impact on microstructure and fuel-swelling performance. Even though various fabrication methods were used, we found little correlation between fabrication variation and fuel swelling. This insensitive relationship between fabrication variation and fuel swelling is primarily due to inhomogeneous microstructures that formed during casting and grain refinement that occurred during rolling. We conclude that the fabrication processes we examined produced similar microstructures, indicating that the fuel microstructure is somewhat insensitive to the fabrication parameters evaluated. However, the relatively small amount of historic data, such as those for grain sizes, limited this analysis. More recently fabricated materials, such as those from ongoing irradiation experiment, Mini-Plate-1 and Mini-Plate-2, were also excluded from this analysis and are intended to be reviewed separately. The findings, that fuel microstructure is somewhat insensitive to the fabrication parameters, do not imply that any fabrication method is acceptable, given the uncertainties in data and fuel-swelling observations. For example, only arc melting and vacuum induction melting casting processes were previously explored in the historic fabrication efforts. In conclusion, the findings should not be extrapolated to other casting processes.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

An integrated two-dimensional modeling method for predicting ductility of thin-walled die cast magnesium

In this paper, a two-dimensional (2D) microstructure-based modeling method is developed in order to predict the ductility of a thin-walled high pressure die cast magnesium (Mg) by considering the three-dimensional (3D) thru-thickness pore distributions. For this purpose, a series of 3D synthetic microstructure-based finite element models and the corresponding 2D models are first generated with various pore volume fractions, pore size distributions and pore shapes. The input material properties for the 2D models are determined based on the 3D cubic model with a spherical pore and the generalized Neuber’s rule. Based on the resulting ductility of the 3D and 2D models, a 3D/2D ductility correlation curve is developed as a function of the characteristics/shape of the input fracture strain curve used in the 3D model. The validity of the ductility correlation curve is examined with casting samples with actual microstructures. Here, the results show that the suggested 2D modeling methodology can be used together with the ductility correlation curve in predicting the ductility of thin-walled Mg castings.

36 MATERIALS SCIENCE↗

Characterization of room temperature recrystallization kinetics in electroplated copper thin films with concurrent x-ray diffraction and electrical resistivity measurements

Concurrent in-situ four-point probe resistivity and high resolution synchrotron x-ray diffraction measurements were used to characterize room temperature recrystallization in electroplated Cu thin films. The x-ray data were used to obtain the variation with time of the integrated intensities and the peak-breadth from the Cu 111 and 200 reflections of the transforming grains. The variation of the integrated intensity and resistivity data with time was analyzed using the Johnson-Mehl-Avrami-Kolmogorov (JMAK) model. For both 111-textured and non-textured electroplated Cu films, four-point probe resistivity measurements yielded shorter transformation times than the values obtained from the integrated intensities of the corresponding Cu 111 reflections. In addition, the JMAK exponents fitted to the resistivity data were significantly smaller. These discrepancies could be explained by considering the different material volumes from which resistivity and diffraction signals originated, and the physical processes which linked these signals to the changes in the evolving microstructure. Based on these issues, calibration of the resistivity analysis with direct structural characterization techniques is recommended.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Pressure-induced stiffness of Au nanoparticles to 71 GPa under quasi-hydrostatic loading

The compressibility of nanocrystalline gold (n-Au, 20 nm) has been studied by x-ray total scattering using high-energy monochromatic x-rays in the diamond anvil cell under quasi-hydrostatic conditions up to 71 GPa. The bulk modulus, K 0 , of the n-Au obtained from fitting to a Vinet equation of state is ~196(3) GPa, which is about 17% higher than for the corresponding bulk materials (K 0 : 167 GPa). At low pressures (<7 GPa), the compression behavior of n-Au shows little difference from that of bulk Au. With increasing pressure, the compressive behavior of n-Au gradually deviates from the equation of state (EOS) of bulk gold. Analysis of the pair distribution function, peak broadening and Rietveld refinement reveals that the microstructure of n-Au is nearly a single-grain/domain at ambient conditions, but undergoes substantial pressure-induced reduction in grain size until 10 GPa. The results indicate that the nature of the internal microstructure in n-Au is associated with the observed EOS difference from bulk Au at high pressure. Full-pattern analysis confirms that significant changes in grain size, stacking faults, grain orientation and texture occur in n-Au at high pressure. We have observed direct experimental evidence of a transition in compressional mechanism for n-Au at ~20 GPa, i.e. from a deformation dominated by nucleation and motion of lattice dislocations (dislocation-mediated) to a prominent grain boundary mediated response to external pressure. In conclusion, the internal microstructure inside the nanoparticle (nanocrystallinity) plays a critical role for the macro-mechanical properties of nano-Au.

high pressure DAC↗

Evaluation of microstructure anisotropy on room and medium temperature ECAP deformed F138 steel

The microstructure developed during severe plastic deformation results in improved mechanical properties because of the decrease in domain sizes and accumulation of defects, mainly dislocation arrays. The characteristic deformation stages observed in low stacking fault energy (SFE) face centered cubic (FCC) materials are highly influenced by the development of the primary and secondary twinning that compete with dislocation glide. In this paper, a low SFE F138 stainless steel is deformed by equal channel angular pressing (ECAP) up to 4 passes at room temperature (RT) and at 300 °C to compare the grain refinement and twin boundary development with increasing deformation. Tensile tests were performed to determine the deformation stages reached by the material before and after ECAP deformation, and the resulting microstructure was observed by TEM. X-ray diffraction and EBSD, average technique the first and local the second one, were used to quantify the microstructural changes, allowing the determination of diffraction domain sizes, dislocation and stacking fault densities and misorientation indices, which lead to a complete analysis of the deformation introduced in the material, with comparative correlations between various microstructural parameters. - Highlights: • The microstructure of ECAP pressed F138 steel was studied using TEM, EBSD and XRD. • Increasing deformation reduced domain sizes and increased dislocation densities. • Dislocation array compactness and misorientation increased with higher deformation. • Largest dislocation densities, mostly screw, match with simultaneous activation of twins. • Several correlations among microstructural features and parameters have been disclosed.

36 MATERIALS SCIENCE↗