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Kotula, Paul Gabriel

Publications and source records attributed to Kotula, Paul Gabriel.

Advanced Characterization: 3D chemistry and structure at sub-nm resolution

This work has started the process of extending nanometer-scale comprehensive microanalysis to the 3rd dimension by combining full x-ray spectral imaging with previously developed computed tomography techniques whereby we acquire a series of spectral images for a large number of projections of the same specimen in the transmission electron microscope and then analyze the composite computed tomographic spectral image data prior to application of existing tomographic reconstruction software. We have demonstrated a needle-shaped specimen geometry (shape/size and preparation method) by focused ion beam preparation and acquisition and analysis of a complete tomographic spectral image on a test material consisting of fine-grained Ni with sub-10 nm alumina particles.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Deformation behavior of sub-micron and micron sized alumina particles in compression

The ability to integrate ceramics with other materials has been limited due to high temperature (>800°C) ceramic processing. Recently, researchers demonstrated a novel process, aerosol deposition (AD), to fabricate ceramic films at room temperature (RT). In this process, sub-micron 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, knowledge in fundamental mechanisms for ceramic particles to deform and form a dense ceramic film is still needed and is essential in advancing this novel RT technology. In this work, a combination of experimentation and atomistic simulation was used to determine the deformation behavior of sub-micron sized ceramic particles; this is the first fundamental step needed to explain coating formation in the AD process. High purity, single crystal, alpha alumina particles with nominal sizes of 0.3 µm and 3.0 µm were examined. Particle characterization, using transmission electron microscopy (TEM), showed that the 0.3 µm particles were relatively defect-free single crystals whereas 3.0 µm particles 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 0.3µm particles deformed plastically, fractured, and became polycrystalline. Moreover, dislocation activity was observed within these particles during compression. These sub-micron sized Al 2 O 3 particles exhibited large accumulated strain (2-3 times those of micron-sized particles) before first fracture. In agreement with the findings from experimentation, atomistic simulations of nano-Al 2 O 3 particles showed dislocation slip and significant plastic deformation during compression. On the other hand, the micron sized Al 2 O 3 particles exhibited brittle fracture in compression. In situ compression experiments showed 3µm 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.

Sarobol, Pylin↗