RESUMO
Transmission electron microscopy (TEM) is an established tool used for the investigation of defects in materials. Traditionally, diffraction contrast techniques-two-beam bright-field and weak-beam dark-field-have been used to image defects due to contrast sensitivity from weak lattice strains. Use of these methods entail an intricate tilt series of imaging using different diffracting vectors, g, to verify the gâ¢b invisibility criterion relative to the different defect types and habit planes inherent to the material. Recently, the addition of down-zone imaging and STEM imaging has also proven to be effective imaging techniques for defect density analysis. Interest in nanocrystalline (NC) materials, spurred by their conjectured superior properties compared to their coarse-grain counterparts, has been thriving and the investigation of their defect morphologies is essential. Maneuvering within NC samples in the TEM adds another layer of difficulty making the aforementioned techniques not practical for application to specimens with complex microstructures. For this reason, we have devised a protocol for identifying NC grains optimally oriented for quantitative analysis using NanoMegas ASTAR automated crystal orientation mapping (ACOM) in the TEM. In this work, we conduct a series of experiments assessing the effectiveness of conventional two-beam bright-field, weak-beam dark-field, and down-zone STEM imaging. We also evaluate an ACOM-assisted multibeam imaging method and compare defect density results obtained using each technique in an irradiated nanocrystalline Au sample.
RESUMO
Many methods used to produce nanocrystalline (NC) materials leave behind non-equilibrium grain boundaries (GBs) containing excess free volume and higher energy than their equilibrium counterparts with identical 5 degrees of freedom. Since non-equilibrium GBs have increased amounts of both strain and free volume, these boundaries may act as more efficient sinks for the excess interstitials and vacancies produced in a material under irradiation as compared to equilibrium GBs. The relative sink strengths of equilibrium and non-equilibrium GBs were explored by comparing the behavior of annealed (equilibrium) and as-deposited (non-equilibrium) NC iron films on irradiation. These results were coupled with atomistic simulations to better reveal the underlying processes occurring on timescales too short to capture using in situ TEM. After irradiation, NC iron with non-equilibrium GBs contains both a smaller number density of defect clusters and a smaller average defect cluster size. Simulations showed that excess free volume contribute to a decreased survival rate of point defects in cascades occurring adjacent to the GB and that these boundaries undergo less dramatic changes in structure upon irradiation. These results suggest that non-equilibrium GBs act as more efficient sinks for defects and could be utilized to create more radiation tolerant materials in future.
RESUMO
The intermediate voltage electron microscope-tandem user facility in the Electron Microscopy Center at Argonne National Laboratory is described. The primary purpose of this facility is electron microscopy with in situ ion irradiation at controlled sample temperatures. To illustrate its capabilities and advantages a few results of two outside user projects are presented. The motion of dislocation loops formed during ion irradiation is illustrated in video data that reveals a striking reduction of motion in Fe-8%Cr over that in pure Fe. The development of extended defect structure is then shown to depend on this motion and the influence of nearby surfaces in the transmission electron microscopy thin samples. In a second project, the damage microstructure is followed to high dose (200 dpa) in an oxide dispersion strengthened ferritic alloy at 500 degrees C, and found to be qualitatively similar to that observed in the same alloy neutron irradiated at 420 degrees C.
