Publications

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

A novel amorphous silicon oxycarbide dispersion-strengthened (SiOC-DS) austenitic steel has been fabricated via a powder metallurgy process. The microstructure of dispersion particles has been characterized by transmission electron microscopy (TEM) and electron backscatter diffraction (EBSD), revealing that amorphous SiOC nanoparticles with an average particle size of 30 nm were homogeneously distributed in the austenite grains with a sub-micrometer grain size. The high strength and hardness of SiOC-DS may be attributed to grain boundary strengthening, as well as dispersion strengthening via dislocation–particle interactions that were revealed by TEM investigations. In situ ion irradiation experiments showed that amorphous SiOC particles were stable after irradiation of 3.7 dpa, and the SiOC/steel interface can be an effective sink for the annihilation of irradiation defects. The excellent mechanical and irradiation properties of SiOC-DS austenitic steel make it a promising structural material for nuclear applications.

The ability of nanoporous metals to avoid accumulation of damage under ion beam irradiation has been the focus of several studies in recent years. The width of the interconnected ligaments forming the network structure typically is on the order of tens of nanometers. In such confined volumes with high amounts of surface area, the accumulation of damage (defects such as stacking-fault tetrahedra and dislocation loops) can be mitigated via migration and annihilation of these defects at the free surfaces. In this work, in situ characterization of radiation damage in nanoporous gold (np-Au) was performed in the transmission electron microscope. Several samples with varying average ligament size were subjected to gold ion beams having three different energies (10 MeV, 1.7 MeV and 46 keV). The inherent radiation tolerance of np-Au was directly observed in real time, for all ion beam conditions, and the degree of ion-induced damage accumulation in np-Au ligaments is discussed here.

Abstract not provided.

Nanocrystalline metals typically have high fatigue strengths but low resistance to crack propagation. Amorphous intergranular films are disordered grain boundary complexions that have been shown to delay crack nucleation and slow crack propagation during monotonic loading by diffusing grain boundary strain concentrations, which suggests they may also be beneficial for fatigue properties. To probe this hypothesis, in situ transmission electron microscopy fatigue cycling is performed on Cu-1 at.% Zr thin films thermally treated to have either only ordered grain boundaries or amorphous intergranular films. The sample with only ordered grain boundaries experienced grain coarsening at crack initiation followed by unsteady crack propagation and extensive nanocracking, whereas the sample containing amorphous intergranular films had no grain coarsening at crack initiation followed by steady crack propagation and distributed plastic activity. Microstructural design for control of these behaviors through simple thermal treatments can allow for the improvement of nanocrystalline metal fatigue toughness.

Abstract not provided.

Abstract not provided.

Abstract not provided.

The effect of ion irradiation on the microstructure of oxide dispersion strengthened (ODS) MA956 steel, before and after friction stir welding (FSW), was studied. Both the base material (BM) and welded stir zone (SZ) were irradiated with 5 MeV Fe ++ ions at 450 °C up to 25 displacements per atom (dpa). Characterization was performed using scanning transmission electron microscopy (STEM) and atom probe tomography (APT), with particular emphasis on the Y–Al–O dispersoid characteristics and dislocation microstructures. After irradiation, the dispersoids in the BM increased in diameter and decreased in number density, which was explained by an Ostwald ripening mechanism. FSW caused significant coarsening and agglomeration of the dispersoids. After irradiation, both the diameter and number density of the SZ dispersoids increased, which was explained by an irradiation-enhanced diffusion mechanism. Dislocation loop and network behavior was also characterized and large dislocation loops of ≈20 nm diameter formed by 1 dpa in both the BM and SZ samples, whereas the network density remained nearly constant with irradiation.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Metallic particles formed in oxide fuels (e.g., UO2) during neutron irradiation have an adverse impact on fuel performance. A fundamental investigation of particle precipitation is needed to predict the fuel performance and potentially improve fuel designs and operations. This study reports on the precipitation of Mo-dominant β-phase particles in polycrystalline CeO2 (surrogate for UO2) films doped with Mo, Pd, Rh, Ru, and Re (surrogate for Tc). In situ heating scanning transmission electron microscopy indicates that particle precipitation starts at ∼1073 K with a limited particle growth to ∼10 nm. While particle concentration increases with increasing temperature, particle size remains largely unchanged up to 1273 K. There is a dramatic change in the microstructure following vacuum annealing at 1373 K, probably due to phase transition of reduced cerium oxide. At the high temperature, particles grow up to 75 nm or larger with distinctive facets. The particles are predominantly composed of Mo with a body-centered cubic structure (β phase). An oxide layer was observed after storage at ambient conditions. In situ heating X-ray photoelectron spectroscopy reveals an increasing reduction of Ce charge state from 4+ to 3+ in the doped CeO2 film at temperatures from 673 to 1273 K. In situ ion irradiation transmission electron microscopy with 2 MeV Al2+ ions up to a dose of ∼20 displacements per atom at nominally room temperature does not lead to precipitation of visible particles. However, irradiation with 1.7 MeV Au3+ ions to ∼10 dpa at 973 K produces ∼2 nm sized pure Pd particles; Au3+ irradiation at 1173 K appears to result in precipitates of ∼6 nm in size. Some of the defects produced by ion irradiation could be nucleation sites for precipitation, leading to generation of smaller particles with a higher concentration. ©

Energy and cost efficient synthesis pathways are important for the production, processing, and recycling of rare earth metals necessary for a range of advanced energy and environmental applications. In this work, we present results of successful in situ liquid cell transmission electron microscopy production and imaging of rare earth element nanostructure synthesis, from aqueous salt solutions, via radiolysis due to exposure to a 200 keV electron beam. Nucleation, growth, and crystallization processes for nanostructures formed in yttrium(iii) nitrate hydrate (Y(NO3)3·4H2O), europium(iii) chloride hydrate (EuCl3·6H2O), and lanthanum(iii) chloride hydrate (LaCl3·7H2O) solutions are discussed. In situ electron diffraction analysis in a closed microfluidic configuration indicated that rare earth metal, salt, and metal oxide structures were synthesized. Real-time imaging of nanostructure formation was compared in closed cell and flow cell configurations. Notably, this work also includes the first known collection of automated crystal orientation mapping data through liquid using a microfluidic transmission electron microscope stage, which permits the deconvolution of amorphous and crystalline features (orientation and interfaces) inside the resulting nanostructures.

Abstract not provided.

Abstract not provided.

A facility for continuously monitoring the thermal and elastic performance of materials under exposure to ion beam irradiation has been designed and commissioned. By coupling an all-optical, non-contact, non-destructive measurement technique known as transient grating spectroscopy (TGS) to a 6 MV tandem ion accelerator, bulk material properties may be measured at high fidelity as a function of irradiation exposure and temperature. Ion beam energies and optical parameters may be tuned to ensure that only the properties of the ion-implanted surface layer are interrogated. This facility provides complementary capabilities to the set of facilities worldwide which have the ability to study the evolution of microstructure in situ during radiation exposure, but lack the ability to measure bulk-like properties. Here, the measurement physics of TGS, design of the experimental facility, and initial results using both light and heavy ion exposures are described. Lastly, several short- and long-term upgrades are discussed which will further increase the capabilities of this diagnostic.

Strength and ductility are mutually exclusive in metallic materials. To break this relationship, we start with nanocrystalline Zirconium with very high strength and low ductility. We then ion irradiate the specimens to introduce vacancies, which promote diffusional plasticity without reducing strength. Mechanical tests inside the Transmission Electron Microscope reveal about 300% increase in plastic strain after self ion-irradiation. Molecular dynamics simulation showed that 4.3% increase in vacancies near the grain boundaries can result in about 60% increase in plastic strain. Both experimental and computational results support our hypothesis that vacancies may enhance plasticity through higher atomic diffusivity at the grain boundaries.

Nanostructures may be exposed to irradiation during their manufacture, their engineering and whilst in-service. The consequences of such bombardment can be vastly different from those seen in the bulk. In this paper, we combine transmission electron microscopy with in situ ion irradiation with complementary computer modelling techniques to explore the physics governing the effects of 1.7 MeV Au ions on gold nanorods. Phenomena surrounding the sputtering and associated morphological changes caused by the ion irradiation have been explored. In both the experiments and the simulations, large variations in the sputter yields from individual nanorods were observed. These sputter yields have been shown to correlate with the strength of channelling directions close to the direction in which the ion beam was incident. Craters decorated by ejecta blankets were found to form due to cluster emission thus explaining the high sputter yields.

Nanocrystalline metals offer significant improvements in structural performance over conventional alloys. However, their performance is limited by grain boundary instability and limited ductility. Solute segregation has been proposed as a stabilization mechanism, however the solute atoms can embrittle grain boundaries and further degrade the toughness. In the present study, we confirm the embrittling effect of solute segregation in Pt–Au alloys. However, more importantly, we show that inhomogeneous chemical segregation to the grain boundary can lead to a new toughening mechanism termed compositional crack arrest. Energy dissipation is facilitated by the formation of nanocrack networks formed when cracks arrested at regions of the grain boundaries that were starved in the embrittling element. This mechanism, in concert with triple junction crack arrest, provides pathways to optimize both thermal stability and energy dissipation. A combination of in situ tensile deformation experiments and molecular dynamics simulations elucidate both the embrittling and toughening processes that can occur as a function of solute content.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

Abstract not provided.

The National Nuclear Security Administration's Tritium Sustainment Program is responsible for the design, development, demonstration, testing, analysis, and characterization of tritium-producing burnable absorber rods (TPBARs) and their components, in addition to producing tritium for the nation's strategic stockpile. The FY18 call for proposals included the specific basic science research topic, "Demonstration and evaluation of advanced characterization methods, particularly for quantifying the concentration of light isotopes (¹H, ²H, and ⁴He, ⁶Li, and ⁷Li) in metal or ceramic matrices". A project IWO-389859 was awarded to the Ion Beam Lab (IBL) at Sandia-NM in FY18. This reports the success we had in developing and demonstrating such a method: 42 MeV Si^{+ 7} from the IBL' s Tandem was used to recoil these light isotopes into special detectors that separated all these isotopes by simultaneously measuring the energy and stopping power of these reoils. This technique, called Heavy Ion - Elastic Recoil Detection or HI-ERD, accurately measured the enriched 6 Li/Li-total of 0.246 +- 0.016, compared to the known value of 0.239. The isotopes ¹H, ²H, ⁴He, ⁶Li and ⁷Li were also measured. (page intentionally left blank)

Abstract not provided.

Abstract not provided.

Abstract not provided.