PNNL

Abstract

Electron backscatter diffraction (EBSD) is a powerful technique for the surface microstructure analysis. EBSD analysis of cubic yttria-stabilized zirconia (YSZ) in two and three dimensions (2-D, 3-D) is demonstrated using sequential slicing from a focused ion beam (FIB) followed by EBSD mapping to represent 3-D reconstructed high density grain structure with random orientation. The statistics related to accuracy of EBSD band detection shows that probability of accurate grain orientation detection increased significantly when the electron beam energy is increased from 10 kV to 30 kV. As a result of better sampling with increased interaction volume, a disparity between local and average grain orientation angle also exhibited the dependence of the electron beam energy to determine the accuracy of grain orientation. To study the accuracy and quality of EBSD band detection as a function of surface roughness and over layer formation, rapid EBSD measurement tests are performed on (a) YSZ surfaces ion-polished at ion beam energies of 65 nA @ 30 kV and 1 nA @ 30 kV and (b) carbon coated versus uncoated YSZ surfaces. The EBSD results at both 10 kV and 30 kV electron beam energies indicate that EBSD band detection accuracy is negatively affected by surface roughness and amorphous over layer formation.