Publications

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Nickel superalloys with cubic L12 structured γ′ (Ni3(Al, Ti)) precipitates exhibit high strength at high temperatures and excellent corrosion resistance when exposed to water. Unlike prior studies on irradiation damage of other Ni-based superalloys, our study on Rene N4 involves much larger γ′ precipitates, ∼450 nm in size, a size regime where the irradiation-induced disordering and dissolution kinetics and the corresponding mechanical property evolution are unknown. We report that under heavy ion irradiation at room temperature, the submicron-sized γ′ precipitates were fully disordered at ∼0.3 dpa and only later partially dissolved after 75 dpa irradiation. Nanoindentation experiments indicate that the mechanical properties of the alloy change significantly, with a dramatic decrease in hardness, with irradiation dose. Three contributions to the change in hardness were examined: defect clusters, disordering and dissolution. The generation of defect clusters in the matrix and precipitates slightly increased the indentation hardness, while disordering of the submicron-sized γ′ precipitates resulted in a dramatic decrease in the total hardness, which decreased further during the early stages of the intermixing between γ′ precipitates and matrix (<18 dpa). Controlling the long-range-ordering and chemical intermixing can be used to tailor the mechanical properties of Ni-based superalloys under irradiation.

The displacement damage induced in W and W-5 wt.% Re and W-5 wt.% Ta alloys by 2 MeV W⁺ irradiation to doses 3.3 × 10¹⁷-2.5 × 10¹⁹ W⁺/m² at temperatures ranging from 300 to 750 °C has been characterised by transmission electron microscopy. An automated sizing and counting approach based on Image J (a Java-based image processing programme developed at the National Institutes of Health) [1] has been performed for all near-bulk irradiation data. In all cases the damage comprised dislocation loops, mostly of interstitial type, with Burgers vectors b = 1/2〈1 1 1〉 (>60%) and b = 〈1 0 0〉. The diameters of loops did not exceed 20 nm with most being ≤6 nm diameter. The loop number density varied between 10²² and 10²³ loops/m³. With increasing irradiation temperature, the loop size distributions shifted towards larger sizes, and there was a substantial decrease in loop number densities. The damage microstructure was less sensitive to dose than to temperature. Under the same irradiation conditions, loop number densities in the W-Re and W-Ta alloys were higher than in pure W but loops were smaller. In grains with normals close to z = 〈0 0 1〉, loop strings developed in pure W at temperatures ≥500 °C and doses ≥1.2 dpa, but such strings were not observed in the W-Re or W-Ta alloys. However, in other grain orientations complex structures appeared in all materials and dense dislocation networks formed at higher doses.

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We study the interplay between the contributions of electron thermal flux and interface scattering to the Kapitza conductance across metal-metal interfaces through measurements of thermal conductivity of copper-niobium multilayers. Thermal conductivities of copper-niobium multilayer films of period thicknesses ranging from 5.4 to 96.2 nm and sample thicknesses ranging from 962 to 2677 nm are measured by time-domain thermoreflectance over a range of temperatures from 78 to 500 K. The Kapitza conductances between the Cu and Nb interfaces in multilayer films are determined from the thermal conductivities using a series resistor model and are in good agreement with the electron diffuse mismatch model. Our results for the thermal boundary conductance between Cu and Nb are compared to literature values for the thermal boundary conductance across Al-Cu and Pd-Ir interfaces, and demonstrate that the interface conductance in metallic systems is dictated by the temperature derivative of the electron energy flux in the metallic layers, rather than electron mean free path or scattering processes at the interface.

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We report on the use of quantitative in situ microcompression experiments in a scanning electron microscope to systematically investigate the effect of self-ion irradiation damage on the full plastic response of <111> Ni. In addition to the well-known irradiationinduced increases in the yield and flow strengths with increasing dose, we measure substantial changes in plastic flow intermittency behavior, manifested as stress drops accompanying energy releases as the driven material transits critical states. At low irradiation doses, the magnitude of stress drops reduces relative to the unirradiated material and plastic slip proceeds on multiple slip systems, leading to quasi-homogeneous plastic flow. In contrast, highly irradiated specimens exhibit pronounced shear localization on parallel slip planes, which we ascribe to the onset of defect free channels normally seen in bulk irradiated materials. Our in situ testing system and approach allows for a quantitative study of the energy release and dynamics associated with defect free channel formation and subsequent localization. As a result, this study provides fundamental insight to the nature of interactions between mobile dislocations and irradiation-mediated and damage-dependent defect structures.

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Localized corrosion of Cu and Al thin films exposed to aqueous NaCl solutions was studied using liquid cell transmission electron microscopy (LCTEM). We demonstrate that potentiostatic control can be used to initiate pitting and that local compositional changes, due to focused ion beam implantation of Au+ ions, can modify the corrosion susceptibility of Al films. This journal is

The progressive build up of fission products inside different nuclear reactor components can lead to significant damage of the constituent materials. We demonstrate the use of time-domain thermoreflectance (TDTR), a nondestructive thermal measurement technique, to study the effects of radiation damage on material properties. We use TDTR to report on the thermal conductivity of optimized ZIRLO, a material used as fuel cladding in nuclear reactors. We find that the thermal conductivity of optimized ZIRLO is 10.7 ± 1.8 W m^-1 K^-1 at room temperature. Furthermore, we find that the thermal conductivities of copper-niobium nanostructured multilayers do not change with helium ion irradiation doses of 10¹⁵ cm^-2 and ion energy of 200 keV, demonstrating the potential of heterogeneous multilayer materials for radiation tolerant coatings. Finally, we compare the effect of ion doses and ion beam energies on the measured thermal conductivity of bulk silicon. Our results demonstrate that TDTR can be used to quantify depth dependent damage.

Transmission electron microscopy (TEM) is a valuable methodology for investigating radiation-induced microstructural changes and elucidating the underlying mechanisms involved in the aging and degradation of nuclear reactor materials. However, the use of electrons for imaging may result in several inadvertent effects that can potentially change the microstructure and mechanisms active in the material being investigated. In this study, in situ TEM characterization is performed on nanocrystalline nickel samples under self-ion irradiation and post irradiation annealing. During annealing, voids are formed around 200 °C only in the area illuminated by the electron beam. Based on diffraction patterns analyses, it is hypothesized that the electron beam enhanced the growth of a NiO layer resulting in a decrease of vacancy mobility during annealing. The electron beam used to investigate self-ion irradiation ultimately significantly affected the type of defects formed and the final defect microstructure.

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A new open-source project evaluation tool, entitle the Materials Engineering Tetrahedron (MET), has been developed to determine the economic viability of materials design, selection, processing, and validation costs associated with any infrastructure-based project. MET improves project design by providing an economic perspective to the traditional materials science tetrahedron, relating microstructure, processing, property, and performance through the introduction of value-based economic costs for each side of the tetrahedron. The resulting size and distortion, from a regular tetrahedron illustrates the balance between the system, component, or material fabrication project detailed. Furthermore, the MET model also allows for increased budget efficiency and the potential for improved identification of cost saving mechanisms.

We investigated the effects of helium ion irradiation energy and sample temperature on the performance of grain boundaries as helium sinks in ultrafine grained and nanocrystalline tungsten. Irradiations were performed at displacement and non-displacement energies and at temperatures above and below that required for vacancy migration. Microstructural investigations were performed using Transmission Electron Microscopy (TEM) combined with either in-situ or ex-situ ion irradiation. Under helium irradiation at an energy which does not cause atomic displacements in tungsten (70 eV), regardless of temperature and thus vacancy migration conditions, bubbles were uniformly distributed with no preferential bubble formation on grain boundaries. Moreover, at energies that can cause displacements, bubbles were observed to be preferentially formed on the grain boundaries only at high temperatures where vacancy migration occurs. Under these conditions, the decoration of grain boundaries with large facetted bubbles occurred on nanocrystalline grains with dimensions less than 60 nm. Finally, we discuss the importance of vacancy supply and the formation and migration of radiation-induced defects on the performance of grain boundaries as helium sinks and the resulting irradiation tolerance of ultrafine grained and nanocrystalline tungsten to bubble formation.

In this study, we demonstrate chemical doping of a topological insulator Bi₂Se₃ using ion implantation. Ion beam-induced structural damage was characterized using grazing incidence X-ray diffraction and transmission electron microscopy. Ion damage was reversed using a simple thermal annealing step. Carrier-type conversion was achieved using ion implantation followed by an activation anneal in Bi₂Se₃ thin films. These two sets of experiments establish the feasibility of ion implantation for chemical modification of Bi₂Se₃, a prototypical topological insulator. Ion implantation can, in principle, be used for any topological insulator. The direct implantation of dopants should allow better control over carrier concentrations for the purposes of achieving low bulk conductivity. Ion implantation also enables the fabrication of inhomogeneously doped structures, which in turn should make possible new types of device designs.

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The reliability of nanomaterials depends on maintaining their specific sizes and structures. However, the stability of many nanomaterials in radiation environments remains uncertain due to the lack of a fully developed fundamental understanding of the radiation response on the nanoscale. To provide an insight into the dynamic aspects of single ion effects in nanomaterials, gold nanoparticles (NPs) with nominal diameters of 5, 20, and 60 nm were subjected to self-ion irradiation at energies of 46 keV, 2.8 MeV, and 10 MeV in situ inside of a transmission electron microscope. Ion interactions created a variety of far-from-equilibrium structures including small (∼1 nm) sputtered nanoclusters from the parent NPs of all sizes. Single ions created surface bumps and elongated nanofilaments in the 60 nm NPs. Similar shape changes were observed in the 20 nm NPs, while the 5 nm NPs were transiently melted or explosively broken apart.

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Here we investigated the microstructural response of various Pd physically vapor deposited films and Er and ErD₂ samples prepared from neutron Tube targets to implanted He via in situ ion irradiation transmission electron microscopy and subsequent in situ annealing experiments. Small bubbles formed in both systems during implantation, but did not grow with increasing fluence or a short duration room temperature aging (weeks). Annealing produced large cavities with different densities in the two systems. The ErD₂ showed increased cavity nucleation compared to Er. The spherical bubbles formed from high fluence implantation and rapid annealing in both Er and ErD₂ cases differed from microstructures of naturally aged tritiated samples. Further work is still underway to determine the transition in bubble shape in the Er samples, as well as the mechanism for evolution in Pd films.

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Radiation-induced segregation (RIS) and subsequent depletion of chromium along grain boundaries has been shown to be an important factor in irradiation-assisted stress corrosion cracking in austenitic face-centered cubic (fcc)-based alloys used for nuclear energy systems. A full understanding of RIS requires examination of the effect of the grain boundary character on the segregation process. Understanding how specific grain boundary structures respond under irradiation would assist in developing or designing alloys that are more efficient at removing point defects, or reducing the overall rate of deleterious Cr segregation. This study shows that solute segregation is dependent not only on grain boundary misorientation, but also on the grain boundary plane, as highlighted by markedly different segregation behavior for the Σ3 incoherent and coherent grain boundaries. The link between RIS and atomistic modeling is also explored through molecular dynamic simulations of the interaction of vacancies at different grain boundary structures through defect energetics in a simple model system. A key insight from the coupled experimental RIS measurements and corresponding defect-grain boundary modeling is that grain boundary-vacancy formation energy may have a critical threshold value related to the major alloying elements' solute segregation. © 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

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An evaluation of calcium tungsten oxide (CaWO4) nanoparticles' properties was conducted using the powders generated from an all-alkoxide solvothermal (SOLVO) route. The reaction involved a toluene/pyridine mixture of tungsten(V) ethoxide ([W(OEt)5]) with calcium bis(trimethyl silyl) amide ([Ca(N(Si(CH3)3)2]) modified in situ by a series of alcohols (H-OR) including neo-pentanol (H-OCH2C(CH 3)3 or H-ONep) or sterically varied aryl alcohols (H-OC6H3R2-2,6 where R = CH3 (H-DMP), CH(CH3)2 (H-DIP), C(CH3)3 (DBP))]. Attempts to identify the intermediates generated from this series of reactions led to the crystallographic identification of [(OEt) 4W(μ-OEt)2Ca(DBP)2] (1). Each different SOLVO generated "initial" powder was found by transmission electron microscopy (TEM) and powder X-ray diffraction (PXRD) to be nanomaterials roughly assigned as the scheelite phase (PDF 00-041-1431); however, these initial powders displayed no luminescent behavior as determined by photoluminescence (PL) measurements. Thermal processing of these powders at 450, 650, and 750 C yielded progressively larger and more crystalline scheelite nanoparticles. Both PL and cathodoluminescent (CL) emission (422-425 and 429 nm, respectively) were observed for the nanomaterials processed at 750 C. Ion beam induced luminescence (IBIL, 478 nm) appeared to be in agreement with these PL and CL measurements. Further processing of the materials at 1000 C, led to a coalescence of the particles and significant improvement in the observed PL (445 nm) and CL measurements; however, the IBIL spectrum of this material was significantly altered upon exposure. These data suggest that the smaller nanoparticles were more stable to radiation effects possibly due to the lack of energy deposits based on the short track length; whereas the larger particles appear to suffer from radiation induced structural defects. © 2013 American Chemical Society.

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Nanocrystalline copper lms were created by both repetitive high-energy pulsed power, to produce material without internal nanotwins; and pulsed laser deposition, to produce nan- otwins. Samples of these lms were indented at ambient (298K) and cryogenic temperatures by immersion in liquid nitrogen (77K) and helium (4K). The indented samples were sectioned through the indented regions and imaged in a scanning electron microscope. Extensive grain growth was observed in the lms that contained nanotwins and were indented cryogenically. The lms that either lacked twins, or were indented under ambient conditions, were found to exhibit no substantial grain growth by visual inspection. Precession transmission elec- tron microscopy was used to con rm these ndings quantitatively, and show that 3 and 7 boundaries proliferate during grain growth, implying that these interface types play a key role in governing the extensive grain growth observed here. Molecular dynamics sim- ulations of the motion of individual grain boundaries demonstrate that speci c classes of boundaries - notably 3 and 7 - exhibit anti- or a-thermal migration, meaning that their mobilities either increase or do not change signi cantly with decreasing temperature. An in-situ cryogenic indentation capability was developed and implemented in a transmission electron microscope. Preliminary results do not show extensive cryogenic grain growth in indented copper lms. This discrepancy could arise from the signi cant di erences in con g- uration and loading of the specimen between the two approaches, and further research and development of this capability is needed.

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The characterization of liposomes was undertaken using in-situ microfluidic transmission electron microscopy. Liposomes were imaged without contrast enhancement staining or cryogenic treatment, allowing for the observation of functional liposomes in an aqueous environment. The stability and quality of the liposome structures observed were found to be highly dependent on the surface and liposome chemistries within the liquid cell. The successful imaging of liposomes suggests the potential for the extension of in-situ microfluidic TEM to a wide variety of other biological and soft matter systems and processes. © 2013 American Chemical Society.

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