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This paper reports on the substantial improvement of specimen quality by use of a low voltage (0.05 to ~1 keV), small diameter (~1 μm), argon ion beam following initial preparation using conventional broad-beam ion milling or focused ion beam. The specimens show significant reductions in the amorphous layer thickness and implanted artifacts. The targeted ion milling controls the specimen thickness according to the needs of advanced aberration-corrected and/or analytical transmission electron microscopy applications.
The consolidation of crystalline powders to obtain dense microstructures is typically achieved through a combination of volume and grain boundary diffusion. In situ transmission electron microscopy was utilized to study neck formation between adjacent nickel particles during the early stages of sintering. It was found that the presence of carbon during consolidation of Ni lowers the reduction temperature of nickel oxides on the particle surface and therefore has the potential to accelerate consolidation. In the absence of carbon, the surface oxides remain present during the early stage of sintering and neck formation between particles is limited by self-diffusion of nickel through the oxide layer. This study provides direct experimental evidence that corroborates related earlier hypotheses of self-cleaning on the surface of the nanoparticles that precedes neck formation and growth.
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