Enhanced radiation tolerance of nanostructured metals is attributed to the high density of interfaces that can absorb radiationinduced defects. Here, cavity evolution mechanisms during cascade damage, helium implantation, and annealing of nanocrystalline nickel are characterized via in situ transmission electron microscopy (TEM). Films subjected to self-ion irradiation followed by helium implantation developed evenly distributed cavity structures, whereas films exposed in the reversed order developed cavities preferentially distributed along grain boundaries. Post-irradiation annealing and orientation mapping demonstrated uniform cavity growth in the nanocrystalline structure, and cavities spanning multiple grains. These mechanisms suggest limited ability to reduce swelling, despite the stability of the nanostructure.
The formation and stability of radiation-induced defects in structural materials in reactor environments significantly effects their integrity and performance. Hydrogen, which may be present in significant quantities in future reactors, may play an important role in defect evolution. To characterize the effect of hydrogen on cascade damage evolution, in-situ TEM self-ion irradiation and deuterium implantation was performed, both sequentially and concurrently, on nickel. This paper presents preliminary results characterizing dislocation loop formation and evolution during room temperature deuterium implantation and self-ion irradiation and the consequence of the sequence of irradiation. Hydrogen isotope implantation at room temperature appears to have little or no effect on the final dislocation loop structures that result from self-ion irradiation, regardless of the sequence of irradiation. Tilting experiments emphasize the importance of precise two-beam conditions for characterizing defect size and structure.
Aerosol deposition (AD) is a solid-state deposition technology that has been developed to fabricate ceramic coatings nominally at room temperature. Sub-micron ceramic particles accelerated by pressurized gas impact, deform, and consolidate on substrates under vacuum. Ceramic particle consolidation in AD coatings is highly dependent on particle deformation and bonding; these behaviors are not well understood. In this work, atomistic simulations and in situ micro-compressions in the scanning electron microscope, and the transmission electron microscope (TEM) were utilized to investigate fundamental mechanisms responsible for plastic deformation/fracture of particles under applied compression. Results showed that highly defective micron-sized alumina particles, initially containing numerous dislocations or a grain boundary, exhibited no observable shape change before fracture/fragmentation. Simulations and experimental results indicated that particles containing a grain boundary only accommodate low strain energy per unit volume before crack nucleation and propagation. In contrast, nearly defect-free, sub-micron, single crystal alumina particles exhibited plastic deformation and fracture without fragmentation. Dislocation nucleation/motion, significant plastic deformation, and shape change were observed. Simulation and TEM in situ micro-compression results indicated that nearly defect-free particles accommodate high strain energy per unit volume associated with dislocation plasticity before fracture. The identified deformation mechanisms provide insight into feedstock design for AD.
Nanostructured metal thin films have been shown to have unique thermal, mechanical, and electrical properties when the internal structure can be maintained. However, this far-from-equilibrium structure has been shown in many cases to be unstable at elevated temperatures. This work investigates the role of surface ledges, large nickel inclusions, electron beam exposure and film thickness on the evolution of high purity, pulsed-laser deposited, free-standing, nickel films via in situ transmission electron microscopy annealing. Grain growth appeared enhanced in a limited temperature range near surface ledges present in the film, but was not affected by large nickel inclusions. In addition, extended exposure to the electron beam resulted in abnormal grain growth. This was hypothesized to be a result of enhanced nickel oxide growth on the surfaces. Finally, increasing film thickness was observed to accelerate the onset of abnormal grain growth and increased the size and number of larger grains. These observations should provide warning that the initial and dynamic surface present in thin films should be taken under consideration during any annealing study, as it may significantly impact the final crystalline structure.
The transient degradation of semiconductor device performance under irradiation has long been an issue of concern. A single high-energy charged particle can degrade or permanently destroy the microelectronic component, potentially altering the course or function of the systems. Disruption of the the crystalline structure through the introduction of quasi-stable defect structures can change properties from semiconductor to conductor. Typically, the initial defect formation phase is followed by a recovery phase in which defect-defect or defect-dopant interactions modify the characteristics of the damaged structure. In this LDRD Express, in-situ ion irradiation transmission microscopy (TEM) in-situ TEM experiments combined with atomistic simulations have been conducted to determine the feasibility of imaging and characterizing the defect structure resulting from a single cascade in silicon. In-situ TEM experiments have been conducted to demonstrate that a single ion strike can be observed in Si thin films with nanometer resolution in real time using the in-situ ion irradiation transmission electron microscope (I3TEM). Parallel to this experimental effort, ion implantation has been numerically simulated using Molecular Dynamics (MD). This numerical framework provides detailed predictions of the damage and follow the evolution of the damage during the first nanoseconds. The experimental results demonstrate that single ion strike can be observed in prototypical semiconductors.
This initial work attempted to determine the feasibility of using advanced in-situ, electron tomography, and precession electron diffraction techniques to determine the structural evolution that occurs during advanced aging of Pd films with nanometer resolution. To date, significant progress has been made in studying the cavity structures in sputtered, evaporated, and pulsed-laser deposited Pd films that result from both the deposition parameters, as well as from He ion implantation. In addition, preliminary work has been done to determine the feasibility of performing precession electron diffraction (PED) and electron tomography in these type of systems. Significant future work is needed to determine the proper conditions such that relevant advanced aging protocols can be developed.