Publications

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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.

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Alloying is often employed to stabilize nanocrystalline materials against microstructural coarsening. The stabilization process results from the combined effects of thermodynamically reducing the curvature-dominated driving force of grain-boundary motion via solute segregation and kinetically pinning these same grain boundaries by solute drag and Zener pinning. The competition between these stabilization mechanisms depends not only on the grain-boundary character but can also be affected by imposed compositional and thermal fields that further promote or inhibit grain growth. In this work, we study the origin of the stability of immiscible nanocrystalline alloys in both homogeneous and heterogeneous compositional and thermal fields by using a multi-phase-field formulation for anisotropic grain growth with grain-boundary character-dependent segregation properties. This generalized formulation allows us to model the distribution of mobilities of segregated grain boundaries and the role of grain-boundary heterogeneity on solute-induced stabilization. As an illustration, we compare our model predictions to experimental results of microstructures in platinum-gold nanocrystalline alloys. Our results reveal that increasing the initial concentration of available solute progressively slows the rate of grain growth via both heterogeneous grain-boundary segregation and Zener pinning, while increasing the temperature generally weakens thermodynamic stabilization effects due to entropic contributions. Finally, we demonstrate as a proof-of-concept that spatially-varying compositional and thermal fields can be used to construct dynamically-stable, graded, nanostructured materials. We discuss the implications of using such concepts as alternatives to conventional plastic deformation methods.

The Fusion Energy Sciences office supported “A Pilot Program for Research Traineeships to Broaden and Diversify Fusion Energy Sciences” at Sandia National Laboratories during the summer of 2021. This pilot project was motivated in part by the Fusion Energy Sciences Advisory Committee report observation that “The multidisciplinary workforce needed for fusion energy and plasma science requires that the community commit to the creation and maintenance of a healthy climate of diversity, equity, and inclusion, which will benefit the community as a whole and the mission of FES”. The pilot project was designed to work with North Carolina A&T (NCAT) University and leverage SNL efforts in FES to engage underrepresented students in developing and accessing advanced material solutions for plasma facing components in fusion systems. The intent was to create an environment conducive to the development of a sense of belonging amongst participants, foster a strong sense of physics identity among the participants, and provide financial support to enable students to advance academically while earning money. The purpose of this assessment is to review what worked well and lessons that can be learned. We reviewed implementation and execution of the pilot, describe successes and areas for improvement and propose a no-cost extension of the pilot project to apply these lessons and continue engagement activities in the summer of 2022.

The dynamic interactions of ions with matter drive a host of complex evolution mechanisms, requiring monitoring on short spatial and temporal scales to gain a full picture of a material response. Understanding the evolution of materials under ion irradiation and displacement damage is vital for many fields, including semiconductor processing, nuclear reactors, and space systems. Despite materials in service having a dynamic response to radiation damage, typical characterization is performed post-irradiation, washing out all information from transient processes. Characterizing active processes in situ during irradiation allows the mechanisms at play during the dynamic ion-material interaction process to be deciphered. In this review, we examine the in situ characterization techniques utilized for examining material structure, composition, and property evolution under ion irradiation. Covering analyses of microstructure, surface composition, and material properties, this work offers a perspective on the recent advances in methods for in situ monitoring of materials under ion irradiation, including a future outlook examining the role of complementary and combined characterization techniques in understanding dynamic materials evolution.

Defects and microstructural features spanning the atomic level to the microscale play deterministic roles in the expressed properties of materials. Yet studies of material evolution in response to environmental stimuli most often correlate resulting performance with one dominant microstructural feature only. Here, the dynamic evolution of swelling in a series of Ni-based concentrated solid solution alloys under high-temperature irradiation exposure is observed using continuous, in situ measurements of thermoelastic properties in bulk specimens. Unlike traditional evaluation techniques which account only for volumetric porosity identified using electron microscopy, direct property evaluation provides an integrated response across all defect length scales. In particular, the evolution in elastic properties during swelling is found to depend significantly on the entire size spectrum of defects, from the nano- to meso-scales, some of which are not resolvable in imaging. Observed changes in thermal transport properties depend sensitively on the partitioning of electronic and lattice thermal conductivity. This emerging class of in situ experiments, which directly measure integrated performance in relevant conditions, provides unique insight into material dynamics otherwise unavailable using traditional methods.

The isotopic composition of water in Earth’s oceans is challenging to recreate using a plausible mixture of known extraterrestrial sources such as asteroids—an additional isotopically light reservoir is required. The Sun’s solar wind could provide an answer to balance Earth’s water budget. We used atom probe tomography to directly observe an average ~1 mol% enrichment in water and hydroxyls in the solar-wind-irradiated rim of an olivine grain from the S-type asteroid Itokawa. We also experimentally confirm that H+ irradiation of silicate mineral surfaces produces water molecules. These results suggest that the Itokawa regolith could contain ~20 l m−3 of solar-wind-derived water and that such water reservoirs are probably ubiquitous on airless worlds throughout our Galaxy. The production of this isotopically light water reservoir by solar wind implantation into fine-grained silicates may have been a particularly important process in the early Solar System, potentially providing a means to recreate Earth’s current water isotope ratios.

The solid-state joining of oxide-dispersion-strengthened (ODS) austenitic steels was achieved using a pulsed electric current joining (PECJ) process. Microstructures of the austenitic grain structures and oxide dispersions in the joint areas were characterized using electron microscopy. Negligible grain growth was observed in austenitic grain structures, while slight coarsening of oxide dispersions occurred at a short holding time. The mechanisms of the PECJ process may involve three steps that occur simultaneously, including the sintering of mechanical alloying powders in the bonding layer, formation of oxide dispersions, and bonding of the mechanical alloying powders with the base alloy. The high hardness and irradiation resistance of ODS alloys were retained in the joint areas. This research revealed the fundamental mechanisms during the PECJ process, which is beneficial for its potential applications during the advanced manufacturing of ODS alloys.

Metal hydrides can store hydrogen isotopes with high volumetric density. In metal tritides, tritium beta decay can result in accumulation of helium within the solid, in some cases exceeding 10 at.% helium after only 4 years of aging. Helium is insoluble in most materials, but often does not readily escape, and instead coalesces to form nanoscale bubbles when helium concentrations are near 1 at.%. Blistering or spallation often occurs at higher concentrations. Radioactive particles shed during this process present a potential safety hazard. This study investigates the effects of high helium concentrations on erbium deuteride (ErD₂), a non-radioactive surrogate material for erbium tritide (ErT₂). To simulate tritium decay in the surrogate, high doses of 120 keV helium ions were implanted into ErD₂ films at room temperature. Scanning and transmission electron microscopy indicated spherical helium bubble formation at a critical concentration of 1.5 at.% and bubble linkage leading to nanoscale crack formation at a concentration of 7.5 at.%. Additionally, crack propagation occurred through the nanocrack region, resulting in spallation extending from the implantation peak to the surface. Electron energy loss spectroscopy was utilized to confirm the presence of high-pressure helium in the nanocracks, suggesting that helium gas plays a predominant role in deformation. This work improves the overall understanding of helium behavior in ErD₂ by using modern characterization techniques to determine: the critical helium concentration required for bubble formation, the material failure mechanism at high concentration, and the nanoscale mechanisms responsible for material failure in helium implanted ErD₂.

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A synthesis process is presented for experimentally simulating modifications in cosmic dust grains using sequential ion implantations or irradiations followed by thermal annealing. Cosmic silicate dust analogues were prepared via implantation of 20–80 ​keV Fe−, Mg−, and O− ions into commercially available p-type silicon (100) wafers. The as-implanted analogues are amorphous with a Mg/(Fe ​+ ​Mg) ratio of 0.5 tailored to match theoretical abundances in circumstellar dusts. Before the ion implantations were performed, Monte-Carlo-based ion-solid interaction codes were used to model the dynamic redistribution of the implanted atoms in the silicon substrate. 600 ​keV helium ion irradiation was performed on one of the samples before thermal annealing. Two samples were thermally annealed at a temperature appropriate for an M-class stellar wind, 1000 ​K, for 8.3 ​h in a vacuum chamber with a pressure of 1 ​× ​10−7 torr. The elemental depth profiles were extracted utilizing Rutherford Backscattering Spectrometry (RBS) in the samples before and after thermal annealing. X-ray diffraction (XRD) analysis was employed for the identification of various phases in crystalline minerals in the annealed analogues. Transmission electron microscopy (TEM) analysis was utilized to identify specific crystal structures. RBS analysis shows redistribution of the implanted Fe, Mg, and O after thermal annealing due to incorporation into the crystal structures for each sample type. XRD patterns along with TEM analysis showed nanocrystalline Mg and Fe oxides with possible incorporation of additional silicate minerals.

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Stainless steel TPBAR components undergo neutron radiation-induced segregation and dislocation loop formation. Comparison experiments with ion beams accelerate the damage, and visualize the damage process with in-situ microscopy. In-situ Au irradiation causes defect formation, but no elemental segregation.

A series of nanopillar compression tests were performed on tungsten as a function of temperature using in situ transmission electron microscopy with localized laser heating. Surface oxidation was observed to form on the pillars and grow in thickness with increasing temperature. Deformation between 850◦C and 1120◦C is facilitated by long-range diffusional transport from the tungsten pillar onto adjacent regions of the Y2O3-stabilized ZrO2 indenter. The constraint imposed by the surface oxidation is hypothesized to underly this mechanism for localized plasticity, which is generally the so-called whisker growth mechanism. The results are discussed in context of the tungsten fuzz growth mechanism in He plasma-facing environments. The two processes exhibit similar morphological features and the conditions under which fuzz evolves appear to satisfy the conditions necessary to induce whisker growth.

A nanostructured oxide-dispersion-strengthened (ODS) CoCrFeMnNi high-entropy alloy (HEA) is synthesized by a powder metallurgy process. The thermal stability, including the grain size and crystal structure of the HEA matrix and oxide dispersions, is carefully investigated by X-ray diffraction (XRD) and electron microscopy characterizations after annealing at 900 °C. The limited grain growth may be attributed to Zener pinning of yttria dispersions that impede the grain boundary mobility and diffusivity. The high hardness is caused by both the fine grain size and yttria dispersions, which are also retained after annealing at 900 °C. Herein, it is implied that the combination of ODS and HEA concepts may provide a new design strategy for the development of thermally stable nanostructured alloys for extreme environments.

Nanostructures with a high density of interfaces, such as in nanoporous materials and nanowires, resist radiation damage by promoting the annihilation and migration of defects. This study details the size effect and origins of the radiation damage mechanisms in nanowires and nanoporous structures in model face-centered (gold) and body-centered (niobium) cubic nanostructures using accelerated multi-cascade atomistic simulations and in-situ ion irradiation experiments. Our results reveal three different size-dependent mechanisms of damage accumulation in irradiated nanowires and nanoporous structures: sputtering for very small nanowires and ligaments, the formation and accumulation of point defects and dislocation loops in larger nanowires, and a face-centered-cubic to hexagonal-close-packed phase transformation for a narrow range of wire diameters in the case of gold nanowires. Smaller nanowires and ligaments have a net effect of lowering the radiation damage as compared to larger wires that can be traced back to the fact that smaller nanowires transition from a rapid accumulation of defects to a saturation and annihilation mechanism at a lower dose than larger nanowires. These irradiation damage mechanisms are accompanied with radiation-induced surface roughening resulting from defect-surface interactions. Comparisons between nanowires and nanoporous structures show that the various mechanisms seen in nanowires provide adequate bounds for the defect accumulation mechanisms in nanoporous structures with the difference attributed to the role of nodes connecting ligaments in nanoporous structures. Taken together, our results shed light on the compounded, size-dependent mechanisms leading to the radiation resistance of nanowires and nanoporous structures.