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DOE OSTI2022

MAGNETIC FLUX EXPULSION IN SUPERCONDUCTING RADIO-FREQUENCY NIOBIUM CAVITIES MADE FROM COLD WORKED NIOBIUM

Trapped residual magnetic field during the cool down of superconducting radio frequency (SRF) cavities is one of the primary sources of RF residual losses leading to lower quality factor. Historically, SRF cavities have been fabricated from high purity fine grain niobium with grain size ~50 to 100 µm as well as large grain with grain size of the order of few centimeters. Non-uniform recrystallization of fine-grain Nb cavities after the post fabrication heat treatment leads to higher flux trapping during the cool down, and hence the lower quality factor. We fabricated two 1.3 GHz single cell cavities from cold-worked niobium from different vendors and processed along with cavities made from SRF grade Nb. The flux expulsion and flux trapping sensitivity were measured after successive heat treatments in the range 800 to 1000°C. The flux expulsion from cold-worked fine-grain Nb cavities improves after 800°C/3h heat treatments and it becomes similar to that of standard fine-grain Nb cavities when the heat treatment temperature is higher than 900°C.

Khanal, B. D.↗

DOE OSTI2022

On-Demand Designing of Cathode Internal Surface Architecture for Dramatic Enhancement of SOFC Performance and Durability

This project is aimed to design and modify the internal surfaces of porous composite cathode from currently commercially viable Solid Oxide Fuel Cells (SOFCs), using additive manufacturing process of Atomic Layer Deposition (ALD). The material systems being investigated are commercial composite electrodes complex three-dimensional topographies. In term of the chemistry of the ALD layer applied on the internal surface of the porous cathode, this project has employed commercially relevant electrolyte, electrocatalyst and noble metal materials set. Such materials are fully compatible with the commercial fuel cells, and this project has developed special nanostructure on the surface of the commercial composite cathodes. The formation of the designed nanoarchitecture on the surface of SOFC cathode has been achieved through precise control of ALD parameters and their effect on overall cell performance and resultant electrochemical reaction mechanism of cathodes has been investigated through full cell electrochemical performance testing and nanostructure characterization by transmission electron microscopy (TEM). Under the support of this award, following has been achieved: (1). For cathode materials in solid oxide fuel cells (SOFCs), such as perovskite mixed conductor La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3-x (LSCF), cation surface segregation and consequently losing conductivity and active sites for the oxygen reduction reaction (ORR) are problematic. To mitigate the cation segregation and enhance SOFC durability, further decorating the internal backbone surface using the desired electrocatalysts could be a promoting approach. Commonly, the cation segregation such as Sr is very volatile, so the effective surface decoration is ideally conformal. Nevertheless, the conformal surface coating would inevitably alter the ORR pathways that initially take place on the surface of the backbone. To reveal the impact of the conformal coating on both the catalytic activity and the conductivity of the cathode, the unary electrocatalyst of Pt or CoO x , was applied to the LSCF/SDC composite electrode of inherently functional SOFCs, respectively. Both ALD coating layers evolve strong interaction with the LSCF composite cathode. Upon operations, the Pt coating layer remains conformal on LSCF grain surfaces but turns into discrete particles on SDC grain surfaces. Meanwhile, CoO x conformal coating grows to be the discrete nanograins on both the LSCF and SDC grains. ALD coating of the cathode alone reduces the ohmic resistance up to 28 % for the entire cells. The increased conductivity induced by the ALD coating of Pt or CoO x is ascribed to different mechanisms. For the inherent functional SOFCs, the present study presents a novel and feasible approach to apply a conformal, dense coating layer on the surface of a mixed conductor, simultaneously increasing the conductivity and durability of the SOFC cathode. (2). High resistance of the oxygen electrode still significantly hinders the state-of-the-art Solid Oxide Fuel Cells (SOFCs). In particular, for an oxygen electrode consisting of mixed electronic and ionic conductors, such as perovskite lanthanum strontium cobalt ferrite (LSCF), it deteriorates due to its low chemical stability of the grain surface. Such degradation is often associated with the segregation of cations. To prevent the cation surface segregation and its resultant perovskite phase decomposition, we demonstrate a conformal ultra-thin (7-10 nm) surface heterogeneous coating layer consisting of subjacent discrete Pt nanoparticles capped with a superjacent fully dense conformal CoO x layer. The performance studies indicate the ALD coating reduces the cell series resistance by up to 40 %. The conformal CoO x layer consists of randomly orientated but single-layered nanograins, with high-density intergranular and surface grain boundaries serving as the electrochemical reaction sites and facilitating mass transport. The conformal coating layer appears to have successfully suppressed the Sr outward diffusion and confined the Sr enriched layer to a ~ 2 nm interface perovskite phase between the coating layer and the LSCF grain surface. Moreover, this ultra-thin Sr enriched perovskite layer presumably possesses high oxygen vacancy and high ionic conductivity and further imposes tensile strain to the LSCF grain surfaces. With the combination of a conformal CoO x nanoionics, Sr enriched layer, and its strained interface, the ALD coating induced surface layer is estimated to have a conductivity of ~ 1.27x10 4 S/cm, which is over two orders magnitude of that from LSCF at 750 ºC.

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2020

Preliminary Study of Potential Utilization of Triassic Rift Basins for Long-Term Carbon Sequestration

Triassic rift basins of the eastern United States present a potential option for long–term carbon dioxide (CO 2 ) sequestration. Exposed and buried basins are located near large point CO 2 sources. Because of their similar origins, comparable fill successions indicate a level of reproducibility that can be conveyed between basins. The thick rock successions of the exposed Culpeper and Gettysburg basins served as proxies for understanding of the basin sequences. Their study allowed recognition of five mappable assemblages of rock types, herein termed lithofacies associations. These lithofacies associations were formed by alluvial fan, braided and meandering streams and marginal and distal lake depositional processes.Stratigraphic architecture of the lithofacies associations within exposed basins suggests a vertical succession that consists of an initial coarse-grained fluvial succession that is progressively replaced upward and basinward by finer grained lacustrine deposits. Along the faulted margins of the basins alluvial fans transitioning to fluvial delta deposits reflect lateral progradation and contemporaneous lateral components of the basin filling.To test the model devised in exposed basins, facies associations were developed for the buried Taylorsville Basin. This basin preserves over 8,000 feet of Triassic rocks that are concealed beneath more than 2,000 feet of Cretaceous and Tertiary Coastal Plain sediments. Composition and stratigraphic architecture of these rocks are similar to those observed in exposed basins. Infilling of the basin was the result of vertical aggradation and lateral progradation of coarse-grained to fine-grained facies. Based upon study of outcrops in the Culpeper and Gettysburg basins, groups of recurring lithologic facies were identified as the fundamental constructs of the basin’s sediment infilling. These groups of facies, termed lithofacies associations, represent an amalgamation of lithologic components from broadly similar depositional systems. These lithologic associations were then extrapolated into the exposed and buried portions of the Taylorsville basins. This effort determined that Triassic rift basins provide several avenues for potential study of geologic sequestration of carbon. The characteristic rift basin succession in the basins presents possible reservoir targets within the marginal fluvial deposits. Furthermore, intrusive and extrusive mafic bodies present a potential source of fracture porosity that could serve as CO 2 reservoirs. Porosity values from thin section analysis of exposed basin samples are higher in alluvial fan and braided fluvial lithofacies. Porosity is highest in samples that show less compaction, due to a lack of ductile lithic fragments and/or higher stratigraphic position. Log data from the Taylorsville Basin indicates that porosity and permeability values in basin marginal fluvial strata are elevated. Near the center of the basin, porosity and permeability values are greatly reduced, primarily owing to the fine-grained character of the lacustrine deposits. Some Triassic basins also contain thick intervals of concordant extrusive and intrusive mafic igneous rocks. These igneous bodies are potential CO 2 reservoirs for several reasons. Firstly, extrusive lava flows provide potential storage in the layers of primary porosity that occur in the vesicules formed at the top of lava flows. Secondly, both lava flows and subsurface igneous sills exhibit extensive fracture porosity produced by the rapid cooling of the flows and intrusions. Thirdly, these igneous rocks are mafic in composition, and studies have shown that iron- and magnesium-rich mafic rocks provide sequestration opportunities through carbonate remineralization. Lastly, extrusive and intrusive igneous rocks are invariably preserved within fine-grained lake deposits. These lacustrine sediments can serve as a fine-grained confining layer that encases the igneous rocks both above and below.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2022

MAGNETIC FLUX EXPULSION IN SUPERCONDUCTING RADIO-FREQUENCY NIOBIUM CAVITIES MADE FROM COLD WORKED NIOBIUM

Khanal, B. D.↗

DOE OSTI2021

Theoretical Analysis of Experimental Data of Sodium Diffusion in Oxidized Molybdenum Thin Films

In this work, the diffusion process of sodium (Na) in molybdenum (Mo) thin films while it was deposited on soda lime glass (SLG) was studied. A small amount of oxygen was present in the chamber while the direct-current (DC) magnetron sputtering was used for the deposition. The substrate temperatures were varied to observe its effect. Such molybdenum films, with or without oxidations, are often used in thin film solar cells, either as back contact or as hole transport layers. Secondary ion mass spectrometry (SIMS) was used to quantify the concentration of the species. A grain diffusion mechanistic model incorporating the effect of grain and grain boundary geometrical shape and size was developed. The model was used to provide an in-depth theoretical analysis of the sodium diffusion in molybdenum thin films that lead to the measured SIMS data. It was observed that not only diffusion coefficients should be considered when analyzing diffusion processes in thin films but also the ratio of grain boundary size to grain size. Both depend on substrate temperature and directly affect the amount of diffused species in the film. The data were analyzed under the light of the film growth speed versus diffusion front speed, the effect of oxygen content, and the effect of substrate temperature on the overall diffusion process. The temperature inversely affects the ratio of grain boundary size and grain size and directly affects the diffusion coefficient, which leads to a preferable temperature at which the highest amount of alkali can be found in the film.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Understanding Uncertainty in Microstructure Evolution and Constitutive Properties in Additive Process Modeling

Coupled process–microstructure–property modeling, and understanding the sources of uncertainty and their propagation toward error in part property prediction, are key steps toward full utilization of additive manufacturing (AM) for predictable quality part development. The OpenFOAM model for process conditions, the ExaCA model for as-solidified grain structure, and the ExaConstit model for constitutive mechanical properties are used as part of the ExaAM modeling framework to examine a few of the various sources of uncertainty in the modeling workflow. In addition to “random” uncertainty (due to random number generation in the orientations and locations of grains present), the heterogeneous nucleation density N 0 and the mean substrate grain spacing S 0 are varied to examine their impact of grain area development as a function of build height in the simulated microstructure. While mean grain area after 1 mm of build is found to be sensitive to N 0 and S 0 , particularly at small N 0 and large S 0 (despite some convergence toward similar values), the resulting grain shapes and overall textures develop in a reasonably similar manner. As a result of these similar textures, ExaConstit simulation using ExaCA representative volume elements (RVEs) from various permutations of N 0 , S 0 , and location within the build resulted in similar yield stress, stress–strain curve shape, and stress triaxiality distributions. It is concluded that for this particular material and scan pattern, 15 layers is sufficient for ExaCA texture and ExaConstit predicted properties to become relatively independent of additional layer simulation, provided that reasonable estimates for N 0 and S 0 are used. However, additional layers of ExaCA will need to be run to obtain mean grain areas independent of build height and baseplate structure.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Modeling the Far-infrared Polarization Spectrum of a High-mass Star-forming Cloud

The polarization spectrum, or wavelength dependence of the polarization fraction, of interstellar dust emission provides important insights into the grain alignment mechanism of interstellar dust grains. We investigate the far-infrared polarization spectrum of a realistic simulated high-mass star-forming cloud under various models of grain alignment and emission. We find that neither a homogeneous grain alignment model nor a grain alignment model that includes collisional dealignment is able to produce the falling spectrum seen in observations. On the other hand, we find that a grain alignment model with grain alignment efficiency dependent on local temperature is capable of producing a falling spectrum that is in qualitative agreement with observations of OMC-1. For the model most in agreement with OMC-1, we find no correlation between the temperature and the slope of the polarization spectrum. However, we do find a positive correlation between the column density and the slope of the polarization spectrum. We suggest this latter correlation to be the result of wavelength-dependent polarization by absorption.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2022

Modeling Chemo-Mechanics with Electrolyte Infiltration to Quantify Degradation of Cathode Particles

One of the main goals in modeling lithium-ion batteries is to improve/predict longevity and resilience of new chemistries. To that end, this talk investigates the formation of stress-induced fracture within polycrystalline cathode particles and the impact on capacity loss. Physically based cathode aging dynamics is simulated in a 3D, continuum-level chemo-mechanical model. The model captures anisotropic Li diffusion within a single polycrystalline particle comprised of hundreds to thousands of randomly oriented grains. A recent addition to this model includes electrolyte infiltration, which occurs when the electrolyte seeps into surface cracks within the particle. The model predicts that particle fracture is primarily due to non-ideal grain interactions with slight dependence on high-rate charge demands. Essentially, when neighboring grains are misaligned, they expand a different rates relative to one another leading to high stresses and ultimately the formation of intraparticle cracks. The model predicts that small particles with large grains develop significantly less damage than larger particles with small grains. Finally, the model predicts most of the chemo-mechanical damage accumulates in the first charge after formation. This chemo-mechanical "damage saturation" effect indicates that initial particle fracture occurs within the first few cycles, while long-term cathode degradation is not solely chemo-mechanically induced. The principle contribution of this research is the use of an anisotropic chemo-mechanical model to test how particle geometry affect capacity fade, which predicts that particle size has a stronger effect on capacity fade than grain size and ultimately that small particles with large grains have the least capacity fade.

cathode↗

DOE OSTI2020

Use of an Alternative Conceptual Model of Vadose Zone Heterogeneity to Evaluate Past Tank Leaks and Other Unplanned Releases within a Tank Farm at the Hanford Site - 20061

Washington State Department of Ecology (Ecology) requested that U.S. Department of Energy (DOE)-Office of River Protection (ORP) consider an evaluation of effects of fine-grained thin sediment layers on transport with a separate alternative conceptual model in its evaluation of the potential impact of tank leaks and other unplanned releases within the tank farm at the Hanford Site. For this alternative model, Ecology recommended that the model be developed based on the general framework of fine-grained units identified by a stakeholder group in their interpretations of variability in moisture content data collected in the vicinity of Waste Management Area (WMA) C. In discussions with DOE-ORP, Ecology acknowledged that the underlying data and interpretations of the occurrence and lateral continuity of the fine-grained thin layers identified by a stakeholder group are uncertain. However, DOE-ORP agreed to Ecology's recommendation and has provided support for the requested evaluation that involved development of an alternative model based on the general framework of the unpublished report by the stakeholder. DOE-ORP considered this evaluation to be a hypothetical evaluation of vadose zone heterogeneities at WMA C. General observations from the range of simulation cases examined in the evaluation of the effects of hypothetical vadose zone heterogeneities at WMA C are as follows. - The movement of the center of mass of the simulated plumes was generally vertically downward below the source for all simulations, including those that incorporated the hypothetical fine-grained units. - All simulations that incorporated hypothetical heterogeneity produced additional plume spreading over what was produced in simulations using Equivalent Homogeneous Media (EHM) model(s)a. The spreading resulted in a broadening of the fringes of the plume, resulting in a wider region of low concentration, but lower peak concentrations associated with the center of mass of the plume. - Simulations that used the silty-sand hydraulic properties, suggested by Ecology for the hypothetical fine-grained units, generally produced similar spreading and slightly lower peak mass flux at the water table when compared to the EHM modeling results. a The EHM-based models used at WMA C do not explicitly include small-scale fine-grained heterogeneities used in the model advocated by Ecology. - Simulations that used the silty-sand hydraulic properties, suggested by Ecology for the hypothetical fine-grained units, generally produced less spreading and an earlier arrival of mass flux at the water table when compared to the use of another set of hydraulic properties from a silty-sand sample collected at a nearby disposal facility. - The EHM representation of the vadose zone generally produced higher peak mass flux and an earlier occurrence of peak fluxes at the water table compared to all analyses incorporating additional hypothetical heterogeneity. Results of this alternative model evaluation of past leaks provided some insight into the transport effects of vadose zone heterogeneities at WMA C that helped resolve Ecology's comments and issues related to the effects of vadose zone heterogeneities on past leaks and losses from the WMA C tank farms area. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

In situ irradiation of spent nuclear fuels

To improve the economics of commercial nuclear reactors, nuclear vendors and utilities are seeking approval for increased burnup usage of the existing nuclear fleet. This is especially critical for meeting the clean energy initiative by the United States Government, Department of Energy (DOE). However, one of the key challenges the nuclear industry faces in this regard is that the regions exposed to high burnup and low temperatures exhibit a fine-grained microstructure with large bubbles known as high-burnup structure (HBS) [1]. The formation of HBS has been correlated to the diminished performance of the reactor, as well as fuel fragmentation and pulverization during transient and accidental conditions [2]. Therefore, it is paramount to understand the mechanisms for HBS formation along with its impact on the properties and performance of nuclear fuels. While existing programs, such as Nuclear Energy Advanced Modeling and Simulation (NEAMS) and Advanced Fuel Campaign (AFC) are focusing on evaluating the performance impact of HBS, the physical mechanisms contributing to HBS formation are still not fully understood. In addition, having predictive capabilities and sound understanding of the microstructural evolution of nuclear fuel is essential for accelerated development, qualification, and deployment of new nuclear materials and novel reactor designs for advanced nuclear reactors. There is a lack of consensus among researchers regarding the mechanisms leading to such restructuring observed in HBS. Grain subdivision due to polygonization versus recrystallization, continuous versus discrete recrystallization occurring in tandem or conjunction, etc., have been proposed and debated. In general, it is hypothesized that defect accumulation and dislocation interaction within the grains cause the realignment of dislocations into grain boundaries, leading to the new subgrain formation, which over time transforms into new grains. However, due to the lack of transient data, the importance of fission rate, irradiation, thermal, and stress history of the fuel on the restructuring could not be assessed. In situ microstructural evolution under various irradiation conditions is desired to bridge this gap. Alternatively, phase-field-based models have been developed to capture HBS formation via discrete recrystallization utilizing the classical nucleation approach [3–5]. However, in these models, the grain nucleation criteria are often defined based on empirical relations for burnup and fission gas density leading to dislocation density change. A mechanistic approach to capture the dislocation interaction with the microstructural features leading to grain subdivision is lacking.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Microstructure evolution of gadolinium doped cerium oxide under large thermal gradients

In this report the effects of large thermal gradient annealing on the microstructure of 10 mol% gadolinium doped ceria (GDC) were investigated. GDC powder was prepared by solvent deficient method and sintered at 1650 °C for 10 h to achieve dense ceramics with ~8 μm grain size. The densified GDC samples were subsequently annealed using a 60 W infrared laser at over 2100 °C for 1 h under a thermal gradient equivalent to ~0.3–0.5 °C/μm. The post-annealed samples at 2150 °C for 1 h exhibit grains with average length and width of 37 and 28 μm, respectively. Electron backscattered diffraction (EBSD) analysis revealed that the post-annealed sample at 2150 °C consists of grains oriented close to five principal directions (<4 3 10>, <0 0 1> and <13 1 14> on [0 0 1], and <7 6 20> and <7 2 7> on [0 1 0]) within a tolerance angle of ±10°, whereas the grains of the pre-annealed sample are randomly oriented. Gadolinium diffuses 20–30 μm away from the irradiated surface, with the measured composition of regions deeper than 30 μm, Ce 0.86 Gd 0.14 O 1.93 , is close to that of the pre-annealed sample, Ce 0.87 Gd 0.13 O 1.94 . Enhancement of total conductivity of the post-annealed GDC (1.1 × 10 -3 S cm -1 at 500 °C, and 2.1 × 10 -2 S cm -1 at 700 °C) is observed when compared to the pre-annealed GDC (3.1 × 10 -5 S cm -1 at 500 °C, and 1.7 × 10 -3 S cm -1 at 700 °C), and points to the decrease in the grain boundary (GB) resistivity. This could be attributed to both the change in GB area and grain alignment.

36 MATERIALS SCIENCE↗

DOE OSTI2023

ac susceptibility studies of intra- and intergrain properties of high-$J_c$ Bi-2212 wires

Bi 2 Sr 2 CaCu 2 O x (Bi-2212) is the only high-$T_c$ superconductor (HTS) available as a multifilamentary round wire with multiple architectures and it is a very promising conductor for the realization of high-field applications. Despite their relatively simple wire fabrication by the powder-in-tube technique, Bi-2212 wires require a tightly controlled overpressure heat treatment (HT) with a multi-parameter time-temperature schedule to achieve high critical current density, $J_c$. Further, the variation of these HT parameters, changes in the wire design, wire diameter and powder quality can lead to variations in both the microstructure and the superconducting performance. Particularly noticeable are variations in $J_c$ performance and degree of filament bridging. In this work, we focus on the use of different magnetic characterization techniques to estimate the bridging level and assess the balance of INTER-grain and intra-grain superconducting properties including the irreversibility field ($H_{\text{irr}}$) and the pinning energy ($U_0$) in differently processed wires. Regardless of the actual bridging level, we find that the supercurrent flows at the filament bundle level, not just at the individual filament level. Moreover, using AC susceptibility we identify two distinct supercurrent contributions, one related to the intra-grain and one to the INTER-grain properties, whose irreversibility fields are different but without large sample-to-sample variation. Moreover, an additional component of intra-grain pinning mechanism becomes effective at low temperatures with positive effects also on the INTER-grain performance. The work clearly shows that detailed magnetic characterizations can become valuable tools to investigate the performance of differently processed Bi-2212 wires, correlating their microstructure and overall transport $J_c$, to obtain a deeper understanding of the causes of performance variation and paths to achieve further improvement.

2212↗

DOE OSTI2021

Sodium doping of solution-processed amine-thiol based CIGS solar cells by thermal evaporation of NaCl

Poor crystallinity, high degree of porosity and rough surfaces are the main drawbacks of solution-processed CIGS absorbers resulting in lower power conversion efficiencies when compared to vacuum-based CIGS solar cells. Therefore, promoting absorber grain growth is key to further improve solution-based solar cell performance. The effect of alkali elements such as Na in CIGS absorbers is generally recognised to have beneficial effects not only on the absorber opto-electronic properties but also on the grain growth. In this work, thermal evaporation of a thin layer of NaCl prior to selenisation resulted in absorbers with significantly larger CIGS grains than previously seen with Na diffusing directly from the from soda-lime glass substrate. NaCl is non-toxic, abundant and readily available compound that has not been typically used as an evaporation source, but rather as an additive into CIGS precursor solution. The effect of Na on these solution-processed CIGS devices was primarily observed in the spectacular morphological changes leading to improved carrier collection and minority carrier lifetimes, but less on the absorber doping. Transmission electron microscopy (TEM) revealed voids forming around large CIGS grains upon NaCl addition and these had a negative effect on inter-grain carrier transport. Nonetheless, the resulting device performance doubled from 5% to 10% with addition of Na using this doping approach; however, a compromise between the optimum grain growth and optimum electronic properties had to be made. This study demonstrates a novel, simple and effective Na-doping strategy for CIGS absorbers and reveals the current limitations of the Na-doping in solution-processed atmospherically deposited cells.

14 SOLAR ENERGY↗

DOE OSTI2021

Thermodynamic stabilization of nanocrystalline aluminum

Nanocrystalline metals are generally unstable due to a large volume fraction of high-energy grain boundaries associated with a small grain size. Preferential dopant segregation to the high-energy grain boundaries is observed to enhance the stability of the material’s microstructure by minimizing its energy. Nanocrystalline aluminum-dopant systems were evaluated for thermodynamic stability against grain growth and phase precipitation via the mechanism of grain boundary segregation according to a modified regular nanocrystalline solution model. Fifty-one potential dopant elements have been evaluated for their efficacy in stabilizing nanostructures with three potential candidates, magnesium, lanthanum, and silicon, identified possessing the characteristics to promote grain boundary segregation and a state of thermodynamic stability in aluminum’s nanocrystalline regime. Here, the minimum dopant content required to achieve nanocrystalline microstructure stability is identified for each of the three candidate elements. Beyond this minimum content, further addition of the dopant elements decreased the final microstructure’s stability with no effects on the existence of a stable nanocrystalline state.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Microstructural refinement in ultrasonically modified A356 aluminum castings

Two A356 aluminum alloys (Al-Si-Mg), one with 0.09 wt.% Fe and one with 0.91 wt.% Fe, were cast in a graphite mold with the simultaneous application of local ultrasonic intensification to refine the as-cast microstructure. Ultrasonication during casting transformed the morphology of primary Al grains from dendritic (~140-290 microns in size) to globular (~33-36 microns in size). The alloy with high Fe exhibited globular grains at distances up to 45 mm away from the ultrasound probe, while the alloy with low Fe exhibited globular grains at distances only up to 6 mm away from the ultrasound probe. Near the location of the ultrasound probe (< 2 mm away), a second non-dendritic microstructural morphology was observed with fine aluminum grains (~9-25 microns in size). This unique fine-grained morphology has not been previously reported, contains a greater concentration of Si relative to the globular microstructure, and may be a large, fully eutectic region. Ultrasonication during casting also transformed the morphology of the ß-Al 5 FeSi phase particles (which are deleterious to the strength and ductility of the alloy) in the high Fe alloy from needle-like to rectangular, which could enable the greater use of secondary Al alloys. Thermodynamic simulations conducted to calculate the solidification paths of the two alloys studied predict that the ß-Al 5 FeSi phase begins to form earlier in the alloy with high Fe. Finally, data suggest that the ß-Al 5 FeSi phase (which is more abundant in alloys with high Fe content) may enhance ultrasonically-induced grain refinement.

36 MATERIALS SCIENCE↗

DOE OSTI2021

In Situ TEM Tensile Testing of Bicrystals with Tailored Misorientation Angles

Grain boundaries have complex structural features that influence strength, ductility and fracture in metals and alloys. Grain boundary misorientation angle has been identified as a key parameter that controls their mechanical behavior, but the effect of misorientation angle has been challenging to isolate in polycrystalline materials. Here, we describe the use of bicrystal Au thin films made using a rapid melt growth process to study deformation at a single grain boundary. Tensile testing is performed on bicrystals with different misorientation angles using in situ TEM, as well as on a single crystalline sample. Plastic deformation is initiated through dislocation nucleation from free surfaces. Grain boundary sliding is not observed, and failure occurs away from the grain boundary through plastic collapse in all cases. The failure behavior in these nanoscale bicrystals does not appear to depend on the misorientation angle or grain boundary energy but instead has a more complex dependence on sample surface structure and dislocation activity.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Reversing inverse Hall-Petch and direct computation of Hall-Petch coefficients

A 2D bicrystal atomistic model of dislocation transmission through a Σ11<101>{131} symmetric-tilt grain boundary reveals details of Hall-Petch breakdown in the single dislocation regime in Al, Ni, and Cu. Partly based on a previous study, this research determines the stress required for a single dislocation to be transmitted through the Σ11 boundary and finds that single dislocation transmission typically deviates from Hall-Petch behavior because the leading partial dislocation becomes trapped in the boundary and emits glissile grain boundary disconnections that cause boundary sliding deformation at stresses well below boundary transmission stresses. Thus, mechanisms of inverse Hall-Petch, namely grain boundary shear and sliding, are shown to operate in lieu of grain boundary transmission in the single dislocation regime. However, by controlling the applied stresses, inverse Hall-Petch can be reversed and typical Hall- Petch grain boundary transmission regained. This, in turn, allows the direct computation of Hall-Petch coefficients. Further, a second dislocation on the same slip plane preserves typical Hall-Petch behavior for Al and Ni and does not lead to boundary sliding events, thus implying a critical grain size for Hall-Petch breakdown based on the pileup model.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Microstructural evolution and intermetallic formation in Zn-3Mg (wt%) powder mixture processed by high-pressure torsion

Severe plastic deformation (SPD) techniques have been used extensively over the past 40 years for producing strong metals and alloys. High-pressure torsion (HPT) is one of the most promising SPD techniques for achieving high strength through nanoscale grain refinement and phase transformation. In this research, a mixture of pure zinc (Zn) and magnesium (Mg) powders, Zn-3Mg (wt%), was HPT-processed under a pressure of 6 GPa for 1, 5, 10, 20, and 30 turns at room temperature to achieve a high strength biodegradable material. In order to understand the effects of pre-consolidation on the resulting microstructure and hardness, HPT processing was performed on loose powders placed in the die and also on a pre-compacted powder mixture and the resulting HPT disks were characterized by X-ray diffraction, scanning electron microscopy, atom probe tomography, and Vickers microhardness. In both cases, the HPT disk microstructures contained nanoscale grains, and stable and metastable strain-induced intermetallics, but an unusual softening appeared at large shear strains. Grain size, grain morphology, and the formation of different intermetallics were analyzed to explain the unusual hardness distribution, and it was found that an inverse Hall-Petch relationship between hardness and grain size exists. It is suggested that thermally-activated phenomena such as grain boundary sliding contributed to the strain-induced softening of this nano-structured biomaterial due to its low melting point. Finally, the current results are compared with those for HPT-processed cast alloys and hybrids of the same composition.

36 MATERIALS SCIENCE↗