Publications

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One of the most common causes of structural failure in metals is fatigue induced by cyclic loading. Historically, microstructure-level analysis of fatigue cracks has primarily been performed post mortem. However, such investigations do not directly reveal the internal structural processes at work near micro- and nanoscale fatigue cracks and thus do not provide direct evidence of active microstructural mechanisms. In this study, the tension-tension fatigue behavior of nanocrystalline Cu was monitored in real time at the nanoscale by utilizing a new capability for quantitative cyclic mechanical loading performed in situ in a transmission electron microscope (TEM). Controllable loads were applied at frequencies from one to several hundred hertz, enabling accumulations of 106 cycles within 1 h. The nanometer-scale spatial resolution of the TEM allows quantitative fatigue crack growth studies at very slow crack growth rates, measured here at ∼10-12 m·cycle-1. This represents an incipient threshold regime that is well below the tensile yield stress and near the minimum conditions for fatigue crack growth. Evidence of localized deformation and grain growth within 150 nm of the crack tip was observed by both standard imaging and precession electron diffraction orientation mapping. These observations begin to reveal with unprecedented detail the local microstructural processes that govern damage accumulation, crack nucleation, and crack propagation during fatigue loading in nanocrystalline Cu.

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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.

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Nanostructuring has been proposed as a method to enhance radiation tolerance, but many metallic systems are rejected due to significant concerns regarding long term grain boundary and interface stability. This work utilized recent advancements in transmission electron microscopy (TEM) to quantitatively characterize the grain size, texture, and individual grain boundary character in a nanocrystalline gold model system before and after in situ TEM ion irradiation with 10 MeV Si. The initial experimental measurements were fed into a mesoscale phase field model, which incorporates the role of irradiation-induced thermal events on boundary properties, to directly compare the observed and simulated grain growth with varied parameters. The observed microstructure evolution deviated subtly from previously reported normal grain growth in which some boundaries remained essentially static. In broader terms, the combined experimental and modeling techniques presented herein provide future avenues to enhance quantification and prediction of the thermal, mechanical, or radiation stability of grain boundaries in nanostructured crystalline systems.

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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.

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An in situ ion irradiation transmission electron microscope has been developed and is operational at Sandia National Laboratories. This facility permits high spatial resolution, real time observation of electron transparent samples under ion irradiation, implantation, mechanical loading, corrosive environments, and combinations thereof. This includes the simultaneous implantation of low-energy gas ions (0.8-30 keV) during high-energy heavy ion irradiation (0.8-48 MeV). Initial results in polycrystalline gold foils are provided to demonstrate the range of capabilities. © 2014 The Authors. Published by Elsevier B.V.

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The ability to integrate ceramics with other materials has been limited due to high temperature (>800degC) ceramic processing. Recently, researchers demonstrated a novel process , aerosol deposition (AD), to fabricate ceramic films at room temperature (RT). In this process, sub - micro n sized ceramic particles are accelerated by pressurized gas, impacted on the substrate, plastically deformed, and form a dense film under vacuum. This AD process eliminates high temperature processing thereby enabling new coatings and device integration, in which ceramics can be deposited on metals, plastics, and glass. However, k nowledge in fundamental mechanisms for ceramic particle s to deform and form a dense ceramic film is still needed and is essential in advancing this novel RT technology. In this wo rk, a combination of experimentation and atomistic simulation was used to determine the deformation behavior of sub - micron sized ceramic particle s ; this is the first fundamental step needed to explain coating formation in the AD process . High purity, singl e crystal, alpha alumina particles with nominal size s of 0.3 um and 3.0 um were examined. Particle characterization, using transmission electron microscopy (TEM ), showed that the 0.3 u m particles were relatively defect - free single crystals whereas 3.0 u m p articles were highly defective single crystals or particles contained low angle grain boundaries. Sub - micron sized Al 2 O 3 particles exhibited ductile failure in compression. In situ compression experiments showed 0.3um particles deformed plastically, fractured, and became polycrystalline. Moreover, dislocation activit y was observed within the se particles during compression . These sub - micron sized Al 2 O 3 particles exhibited large accum ulated strain (2 - 3 times those of micron - sized particles) before first fracture. I n agreement with the findings from experimentation , a tomistic simulation s of nano - Al 2 O 3 particles showed dislocation slip and significant plastic deformation during compressi on . On the other hand, the micron sized Al 2 O 3 particles exhibited brittle f racture in compression. In situ compression experiments showed 3um Al 2 O 3 particles fractured into pieces without observable plastic deformation in compression. Particle deformation behaviors will be used to inform Al 2 O 3 coating deposition parameters and particle - particle bonding in the consolidated Al 2 O 3 coatings.