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At least 775 records · Page 43

Assessing Manufacturability of the Oxide Dispersion Strengthened (ODS) 14YWT Alloy Fuel Cladding Tube Using SolidStir™ Technology

The 14YWT (Fe–14Cr–3W–0.4Ti–0.3Y2O3 (wt.%)) alloy is a potential candidatematerial for fabricating fuel cladding tubes and other structural components to be used in next-generation advanced nuclear reactors. Due to inherent limitations of current processing routes, this research explored a new variant of friction stir processing, commercially referred to as SolidStir™ Extrusion (patent pending) technology from Enabled Engineering to consolidate and extrude 14YWT powder into a fuel cladding tube. Several single-layer and multiple-layer consolidation experiments were carried out in an Inconel 625 die to determine the suitable processing parameters for SolidStir™ extrusion of the 14YWT alloy cladding tube. With these processing parameters, a 16–18 mm long tube of the 14YWT alloy with no visible defects was successfully extruded using this novel technology. Microstructural characterization results obtained using optical microscopy, scanning electron microscopy, energy dispersive spectroscopy, electron backscatter diffraction, and transmission electron microscopy will be presented.

Advanced Materials and Manufacturing Technology↗

Microstructure and fracture toughness characterization of three 9Cr ODS EUROFER steels with different thermo-mechanical treatments

Ferritic martensitic ODS steels are one of the candidate structural materials for future Gen-IV nuclear fission and fusion reactors. Here, the dependence of fracture toughness on microstructure was investigated by comparing three 9Cr ODS EUROFER steels manufactured through different thermo-mechanical processing routes. Quasi-static fracture toughness testing was performed with sub-sized C(T) specimens and microstructural characterization was carried out using scanning electron microscopy, electron backscatter diffraction, and transmission electron microscopy. It was found that at lower test temperatures (-100 – 22 °C), the fracture toughness was primarily controlled by crack initiation at sub-micron particles and by production of secondary cracks during fracture. At higher temperatures (above 100 °C), fracture toughness was predominantly controlled by the matrix ductility and the grain boundary strength with a relatively ductile coarse-grained alloy demonstrating higher fracture toughness compared to high-strength fine-grained alloys. These results and discussion show that variations in thermomechanical treatments can produce significant differences in microstructure and fracture toughness behavior of ferritic martensitic ODS steels.

36 MATERIALS SCIENCE↗

Microstructure analysis of laser beam weldments performed on neutron-irradiated 304L steel containing 3 and 8 appm helium

We report that AISI 304 L austenitic stainless steel is one of the major structural materials used in light water reactors (LWRs). In the future, 304 L components may require repair, and several welding techniques have been proposed as candidates. In this study, laser beam welding using the low-energy contribution approach was performed in ~2016 on neutron-irradiated AISI 304 L steel with nominal values of 3 and 8 appm helium (He). The goal was to investigate the impact of helium on the irradiated material weldability and evaluate helium-associated damage. The weld and heat-affected zone (HAZ) microstructure was studied using scanning electron microscopy, electron backscatter diffraction, and transmission electron microscopy (TEM). Analysis of the weldment cross-sections did not reveal severe cracking. Still, evidence of incipient helium-associated damage was observed in the HAZ, manifesting as degraded grain boundaries (GBs) “decorated” by pore chains and mostly small (i.e., ≤ 25-30 µm) scattered cracks. The largest observed crack was ~50 µm in length. Helium-associated damage was localized within ~200-300 µm of the weld pool boundary, and the fraction of the compromised GBs, as a rule, was below ~9-11% of the total GB network. TEM analysis showed significant annealing of the radiation-induced defects at distances up to ~300 µm from the weld pool boundary. Inside the HAZ, the cavities (likely, helium bubbles) tended to form at GBs and inclusions, such as manganese sulfide precipitates in the grain interior. Crystallography analysis of the HAZ damage showed that random high-angle boundaries were most susceptible to helium-associated damage. In contrast, low-angle random boundaries and twin boundaries appeared to be strongly resistant to degradation from the combined effects of helium and welding.

36 MATERIALS SCIENCE↗

Material flow behavior and microstructural refinement of AA6061 alloy during friction extrusion

In this work we used friction extrusion (FE), a solid phase processing technique, to produce dense, fully consolidated 5?mm rods of aluminum alloy 6061 (AA6061). The combination of large shear stresses and high temperatures at the tool-billet interface during extrusion produced equiaxed, dynamically recrystallized grains and finely distributed precipitates. Texture and microstructure evolution during extrusion was investigated in detail using scanning electron microscopy, electron backscatter diffraction, and transmission electron microscopy. Smoothed particle hydrodynamics simulation was performed to study complex material flow during extrusion. Simulation results suggest spiral material flow during extrusion which corroborated experimental results. Advantages of friction extruded microstructure over conventionally extruded counterparts are also explored using flash annealing for solution treatment followed by artificial aging. Mechanical properties of the as-friction extruded, and the artificially aged specimens were evaluated using tensile testing and compared with conventional extruded material properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Microstructural evolution in shear-punch tests: A comparative study of pure Cu and Cu-Cr alloy

Understanding the mechanisms behind microstructural evolution during shear deformation has been a long-standing area of interest. However, establishing a connection between microstructure, mechanical properties, and extent of shear deformation is challenging and requires refined experimental approaches. Shear-punch testing (SPT) provides a controlled method to introduce shear into small volumes of material that later can be subjected to detailed microstructural characterization. In this study, we utilize an SPT device to induce shear deformation to pure copper and a binary copper-chromium alloy. Electron backscatter diffraction and transmission electron microscopy were used to study the mechanisms of plastic deformation after SPT. Our results indicate that shear deformation of pure Cu produces a dense network of intercepting microshear bands upon sustained deformation. Twin boundaries undergo degradation into high angle grain boundaries due to simultaneous deviation from the axis-angle pair condition of 60° misorientation on [111] direction. The presence of 50% volume Cr particles in the soft Cu matrix fundamentally altered the shear deformation mechanism. Preferential deformation of the Cu matrix led to accelerated shear-induced formation of low and high angle grain boundaries, and subsequent grain refinement. Comparatively, no grain refinement occurred in pure Cu at a strain ~10 times larger (ϵ = 4.73) than that of the copper-chromium case (ϵ = 0.42). Overall, our study sheds light on the microstructural evolution during shear deformation and highlights the significant influence of particle reinforcements on the shear deformation mechanisms of metals.

36 MATERIALS SCIENCE↗

A boundary-based approach to the multiscale microstructural characterization of a W-Ni-Fe tungsten heavy alloy

Here, a combination electron backscattered diffraction and transmission electron microscopy based approach has been implemented to study the effects of purposefully introduced anisotropy in a tungsten heavy alloy (WHA) through hot-rolling. Particular attention has been paid to changes in number and proportion of various boundary types from a quantitative standpoint; incorporating qualitative behavioral observations from prior analyses to generate experimentally-validated bases for the examination and application of a microstructure which exhibits an optimal balance of strength and ductility. It is asserted that a combination of increased temperatures during rolling and additional isothermal hold time for the post-rolling annealing steps may lead to a reduction in unfavorable textural components due to rolling in the W-phase and a decrease in premature fracture due to W-W microcracking respectively. This is expected to further increase the proportion of interphase boundaries and improve the ductility of these rolled structures, producing a superior rolled WHA microstructure.

36 MATERIALS SCIENCE↗

Nucleation and growth of voids in shock loaded copper bicrystals

Understanding the evolution of damage and deformation due to spall at grain boundaries can provide a basis for connecting micro- to macroscale failure behavior in metals under extreme conditions. Copper bicrystal samples were shock loaded using flyer-plate impacts in a light gas gun with shock stresses ranging from 3 to 6 GPa. Pulse duration as well as crystal orientation along the shock direction were varied for a fixed boundary misorientation to determine their effects on void nucleation and coalescence. Samples were soft recovered and cross-sectioned to characterize damage using electron backscattering diffraction and scanning electron microscopy to gather information on damage characteristics at and around the GB, with emphasis on growth of boundary and bulk voids. Chemistry and composition analysis were also performed on samples to determine if trace elements present in a sample affected the threshold for void nucleation. Results show that the kinetics of damage growth at the boundary are strongly affected by stress level and impurities. It was found that the boundary selected had a similar or even lower tendency to show damage than the bulk at low pulse durations and amplitudes. As pulse duration and amplitude increased damage localized at the boundary, which was found to consist of many small voids, indicating that the boundary experienced rapid void nucleation and coalescence. Furthermore, the presence of impurities correlated strongly with scatter on damage evolution.

36 MATERIALS SCIENCE↗

Vitreous silica formation within shear bands in a dynamically compacted granular crystalline α‐quartz

A shear band is a heterogeneous, narrow seam within a solid material whose formation is caused by intense localized shearing when a sufficiently large amount of deformation occurs. If that deformation occurs at a sufficiently rapid rate, with operative friction, then co‐located ephemeral heating will occur in the shear band. In this study, shear bands were produced from dynamic shear‐induced compaction of a granular form of crystalline α‐quartz (SiO 2 ). The produced shear bands were approximately 25‐µm thick and were examined with scanning electron microscopy/electron backscatter diffraction, transmission electron microscopy, Raman spectroscopy, and nanoindentation. Further, they were found to contain a mixture of vitreous silica and small‐sized crystallites. This finding is significant because the presence of the vitreous silica within the shear band is a postmortem indicator that the localized temperature had reached or exceeded the melting temperature (∼1723°C) of crystalline SiO 2 during the rapid shear and compaction and then sufficiently rapid cooling quenched in that vitreous state.

36 MATERIALS SCIENCE↗

Collaborative R&D with REEL Solar Inc (REEL) to Understand and Overcome Performance Limitations in CdTe Solar Cells: Cooperative Research and Development (Final Report)

This CRADA will focus on processing, advanced characterization, and testing of photovoltaic materials and devices to understand and improve REEL CdTe solar technology. This will include examining process variations and different buffer, absorber, and contact layers from REEL and NLR to maximize performance. The unique and diverse advanced characterization tools at NLR, such as time-resolved photoluminescence, capacitance-voltage measurements, electron beam scattered diffraction, cathodoluminescence, electron microscopy, TOF-SIMS, and other measurements will be applied to characterize REEL processing to improve understanding and guide experimental directions. Accelerated stability and potential induced degradation tests will be used to analyze metastability, short-and-long term degradation, and improve bankability. A second and major thrust this period will be joint development of Si/CdTe tandem solar cells to overcome industry wide terrestrial solar efficiency limits with the two lowest cost and manufacturable solar materials today. This will include developing novel transparent back contacts that can be incorporated into tandem structures and other novel solar applications, detailed analysis of designs and configurations for CdTe/Si tandem modules, and prototyping REEL CdTe Technology with Si bottom cells in tandem structures.

14 SOLAR ENERGY↗

Lubrication with sputtered MoS2 films.

Sputtered MoS2 films (2000-6500 A) were deposited on highly polished metal surfaces. These films have a low coefficient of friction (0.03-0.04) at speeds of 40-80 rpm and loads of 250-1000 grams. At loads of 250 grams the wear lives are over 0.5 million cycles, but at 1000 gram loads, it decreases to 38,000 cycles. Friction experiments and tensile tests have indicated that sputtered films have a strong adherence to metal surfaces. Electron transmission, diffraction and scanning electron microscopy show that these films have an extremely small particle size, less than 30 A in diameter, and are very dense and free from observable pinholes. The high kinetic energy of these sputtered species, the submicroscopic particle size and the sputter-etched substrate surface is responsible for strong adhesion and cohesion of the sputtered film.

Spalvins, T.↗

Lubrication with sputtered MoS2 films.

Sputtered MoS2 films (2000-6500 A) were deposited on highly polished metal surfaces. These films have a low coefficient of friction (0.03-0.04) at speeds of 40-80 rpm and loads of 250-1000 grams. At loads of 250 grams, the wear lives are over 0.5 million cycles, but at 1000 gram loads, it decreases to 38,000 cycles. Friction experiments and tensile tests have indicated that sputtered films have a strong adherence to metal surfaces. Electron transmission, diffraction, and scanning electron microscopy show that these films have an extremely small particle size less than 30 A in diameter and are very dense and free from observable pinholes.

Spalvins, T.↗

Mineralogical Study of Hydrated IDPs: X-Ray Diffraction and Transmission Electron Microscopy

Chondritic hydrated interplanetary dust particles (IDPs) comprise up to 50% of all IDPs collected in the stratosphere [1]. Hydrated IDPs are generally believed to be derived from asteroidal sources that have undergone aqueous alteration. However, the high C contents of hydrated IDPs (by 2 to 6X CI levels [2,3]) indicate that they are probably not derived from the same parent bodies sampled by the known chondritic meteorites. Some hydrated IDPs exhibit large deuterium enrichments [4] similar to those observed in anhydrous IDPs. Both anhydrous and hydrated IDPs contain a variety of anhydrous minerals such as silicates, sulfides, oxides, and carbonates. Controversies on hydrated IDPs still exist regarding their formation, history, and relationship to other primitive solar system materials, because of the lack of a systematic series of analysis on individual hydrated IDPs. In this study, we combine our observations of the bulk mineralogy, mineral/ organic chemistry in order to derive a more complete picture of hydrated IDPs.

Nakamura, K.↗

Mechanical twinning of monazite expels radiogenic Pb

Mechanical twins form by the simple shear of the crystal lattice during deformation In order to test the potential of narrow twins in monazite to record the timing of their formation, a ~1,700 Ma monazite grain deformed at ~980 Ma was investigated by electron backscattered diffraction (EBSD), transmission electron microscopy (TEM) and atom probe tomography (APT). APT 208Pb/232Th ages indicate that the twin was entirely reset by radiogenic Pb-loss during its formation at conditions far below the monazite closure temperature. The results are consistent with a model where Pb is liberated during rupture of REE-O bonds in the large REEO9 polyhedra during twinning. Liberated Pb is likely to migrate along fast diffusion pathways such as crystal defects. The combination of a quantitative microstructural investigation and nanogeochronology provides a new approach for understanding the history of accessory phases.

monazite↗

Microstructural Evolution of the Civet Cat Norite (72255)

The ‘Civet Cat Norite’ is a ~ 2.5 cm clast within the Apollo impact melt breccia sample 72255 collected during Apollo 17 EVA 2 at Boulder 1. The norite is primarily composed of plagioclase and orthopyroxene with fine-scale exsolution lamellae of augite. The plagioclase and orthopyroxene (OPX) coexist with minor quartz and augitic clinopyroxene (CPX), and accessory apatite, baddeleyite, chromite, ilmenite, loveringite, merrillite, rutile and zircon. The major minerals range from 1 to 4 mm in size and show a cataclastic texture indicated by banding of the light and dark phases]. The chemical composition of the orthopyroxene, augitic exsolution lamellae, and exsolved oxides suggest the norite crystallized in the lower crust of the Moon (10 – 70 km depth) and was subsequently excavated by impact(s). Shock pressure estimates for the norite range from 15 – 35 GPa based on maskeleynite formation within the plagioclase, kink banding in pyroxenes, and granular recrystallization in the accessory phosphates. Previous Rb-Sr and 40 Ar/ 39 Ar analyses recalculated with modern decay constants yield relatively young ages of 4.16 ± 0.05 Ga and 3.99 ± 0.03 Ga, respectively. However, recent U-Pb analyses of some zircon grains from within the Civet Cat yield an age of 4.45 ± 0.03 Ga. While this is the oldest age for any rock recovered from the Moon, the full age spread of zircon from the Civet Cat range from ca. 4.46 to 4.02 Ga, indicating variable Pb-loss and complicating interpretation of the primary age. Recent atom probe analyses indicate minimal Pb mobilization within the oldest zircon grain from Civet Cat, supporting the interpretation that these ancient zircon ages reflect the age of the norite, rather than an apparent antiquity caused by reverse discordance. To investigate the potential antiquity and deep crustal origin of the Civet Cat norite, we have undertaken high resolution microstructural analyses of the major, minor, and accessory minerals to characterize the primary igneous textures and secondary overprinting by impact and metamorphism. The employed analytical techniques include scanning electron microscope-based electron backscatter diffraction (EBSD) analyses, electron probe microanalyzer (EPMA) chemical analyses, and transmission electron microscopy (TEM) of pyroxene, plagioclase, quartz, zircon, and phosphates.

T M Erickson↗

Characterization of Alloy 709 Commercial Heats

The creep-resistant austenitic stainless steel Alloy 709 (Fe-20Cr-25Ni (wt%) based steel) is being investigated as a candidate structural material for the next generation of advanced reactors. Unlike conventional solid solution strengthened austenitic stainless steels, Alloy 709 develops a variety of precipitates during aging at different temperatures and times. In this study, precipitate evolution during short-term aging at 775°C was characterized. The effect of aging time (e.g., 10 vs. 100 hours) and cooling after aging (e.g., water quench vs. air cool) on grain size and precipitates have been investigated using light optical microscopy (OM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM), and energy-dispersive X-ray spectroscopy (EDS). MX (Ni,Tb)(C,N) and M23C6 (Cr,Mo)C precipitates were observed in all the statically-aged samples. The grain size distribution in the sample aged for 10 hours and water quenched (10Q) versus the one aged for 100 hours and air cooled (100A) were comparable. This indicates that grain structure was fairly stable when aging at 775°C for up to 100 hours. In contrast, the sample aged for 10 hours and air cooled (10A) showed the smallest and the most uniform grain size distribution. This phenomenon was observed in only one sample. More studies on duplicate samples are needed to confirm the results obtained. The cooling medium (e.g., water quench vs. air cool) was not observed to impact the size nor the distribution of the MX and M23C6 precipitates. Increasing the aging time resulted in the following: (1) a decrease in dislocations as well as the number density of small precipitates; (2) an increase in the ratio of free precipitates that were not pinning dislocations; (3) relatively higher N, Nb, and Ti concentration in MX precipitate; (4) some increase in length of M23C6 carbides which were located on the coherent boundaries; and (5) the introduction of Sienriched M6X precipitates. The tensile tests at room temperature showed similar properties for each of the static aging treatments, indicating that the differences observed in the microstructural analysis did not have a significant impact on the tensile properties.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

In situ synchrotron X-ray diffraction analysis of ultrasonically assisted microstructure refinement during laser melting process

This work investigates the effect of ultrasonic treatment (UST) on the microstructure of AA4043 alloy during laser melting process. Here, the study utilizes in situ synchrotron X-ray diffraction (SXRD) and postmortem electron backscatter diffraction (EBSD) techniques to examine the ultrasonic grain refinement mechanism. The SXRD diffraction patterns exhibit higher continuity of major diffraction rings in the UST-test pattern, indicating a more refined grain structure. The presence of new diffraction spots in the post-test diffraction pattern with UST suggests the breakdown of epitaxial growth of columnar dendrites during solidification. Thermal profiles determined by analyzing the lattice parameter evolution show a faster cooling rate with UST. The inverse pole figures and aspect ratio distribution from EBSD reveal that the UST samples exhibit a refined, more equiaxed grain structure along the weld centerline. UST sample also develops more fine-sized low angle grain boundaries (LAGBs). These features offer better hot-cracking resistance in aluminum alloys.

36 MATERIALS SCIENCE↗

X-Ray-Diffraction Tests Of Irradiated Electronic Devices: II

Report describes research on use of x-ray diffraction to measure stresses in metal conductors of complementary metal oxide/semiconductor (CMOS) integrated circuits exposed to ionizing radiation. Expanding upon report summarized in "X-Ray-Diffraction Tests Of Irradiated Electronic Devices: I" (NPO-18803), presenting data further suggesting relationship between electrical performances of circuits and stresses and strains in metal conductors.

Shaw, David C.↗

Investigation of phase-transformation path in TiZrHf(VNbTa)x refractory high-entropy alloys and its effect on mechanical property

Refractory high-entropy alloys (RHEAs) show a great potential as structural materials due to their remarkable properties, such as high strength and thermal stability. Despite these advantages, the RHEAs still suffer from the limited ductility at room temperature. To overcome the strength-ductility trade-off, the new RHEA design strategy, transformation-induced plasticity (TRIP) HEAs, have been developed by applying metastability-engineering approach. With the newly developed RHEAs design strategy, we designed metastable RHEAs, TiZrHfVxNbxTax (x = 1.0, 0.5 and 0.1) with decrease of the β-stabilizing elements (V, Nb, and Ta) to promote the transformation-induced ductility and work-hardening capability. The proper addition of the β-stabilizing elements (V, Nb, and Ta) into the ternary equi-molar TiZrHf alloy (TiZrHfV 0.1 Nb 0.1 Ta 0.1 ) leads to stress/strain-induced phase transformation from the body-centered cubic (BCC) to hexagonal-close-packed (HCP) α' and/or orthorhombic α" phases. Here, detailed studies on the phase transformation sequence during the deformation were carried out using X-ray diffraction (XRD), electron back-scattered diffraction (EBSD), and transmission-electron microscope (TEM), which revealed the stepwise phase transformation that is responsible for the strong strain hardening behavior. Furthermore, we further suggested the new transformation-induced-plasticity (TRIP) HEA design strategy, applying the Bo-Md approach.

36 MATERIALS SCIENCE↗