RESUMEN
Structural ceramics are typically used in polycrystalline form. It is well known that polycrystalline ceramics often show the intergranular fracture. To improve their mechanical properties, transition metals can be used as dopants into a bulk material, which tend to segregate into the grain boundaries[1]. However, the effect of dopant segregation on grain boundary fracture is still uncertain. In order to investigate the fracture behavior of a dopant-segregated grain boundary, we observed the crack propagation of a Zr-doped alumina grain boundary by in situ nanoindentation in a transmission electron microscope (TEM), and characterized the fracture surface by scanning TEM (STEM).An alumina bicrystal with a Zr-doped Σ13 grain boundary was fabricated by diffusion bonding at 1500(o)C for 10 hours in air, where a face of one crystal was coated by Zr metal in advance to the bonding (Fig. 1a). A TEM sample was prepared from the bicrystal by mechanical grinding and Ar ion milling. For in situ indentation, the sample had a free edge perpendicular to the grain boundary (Fig. 1b). The indentation experiment was performed by using a double-tilt indentation holder (Nanofactory) and JEM-2010 (200kV, JEOL). The fracture surface was further observed by high angle annular dark field (HAADF) STEM (ARM-200F, 200kV, JEOL).jmicro;63/suppl_1/i20-a/DFU064F1F1DFU064F1Fig. 1.(a) Schematic illustrations of bicrystal fabrication by diffusion bonding and (b) Bright field TEM image showing the geometric arrangement of the in situ nanoindentation experiment In the in situ TEM nanoindentation experiment, at first a crack was introduced in bulk close to the grain boundary and propagated with the amount of indentation. After the crack reached the grain boundary, it preferentially propagated along the grain boundary. To identify the crack pass at the atomic level, the STEM analysis was performed. We found that three-atomic-layer Zr was formed in the unbroken region of the grain boundary, whereas one to three Zr layers remained on the fracture surface. This indicates that the crack propagated within the segregation region of Zr in the grain boundary. In the presentation, we will discuss the crack propagation behavior and the atomic structure of the fracture surfaces in detail.