Elimination of the charge effect on zirconia coatings using a focused ion beam for characterization of the three-dimensional microstructure

Abstract

How to improve the acquisition efficiency of electron back scatter diffraction (EBSD) and meanwhile avoid the drifting of images caused by the charge effect is still an issue that needs to be solved urgently for three-dimensional (3D) EBSD characterization of non-conductive ceramic materials. The purpose of this study is to solve the problem based on an experimental and theoretical basis using the yttria-stabilized zirconia (YSZ) coating as the research subject. To eliminate the charge effect, the charge equilibrium point of the YSZ coating was determined using the Duane–Hunt limit method. When the incident energy is equal to the E2 value (3.06 keV), the charge effect on the scanning electron microscopy images of the YSZ coating disappears. However, the incident energy of 3.06 keV exhibits lower EBSD collection efficiency for a 3D EBSD result because of the long exposure time; therefore, increasing the incident energy to 7 keV under the large beam current is a practical way to improve EBSD collection efficiency, which inevitably results in the charge problem again. Furthermore, Ga ion implantation caused the charge effect on the YSZ coating at 7 keV under the large beam current to disappear, which can be attributed to the decrease in bandgap widths and the improvement of electrical conductivity of the t-YSZ phase after Ga ion implantation based on first principles. Calculations of the cohesive energies reveal that Ga ions are more likely to occupy the lattice positions of the YSZ coating after Ga ion implantation. Finally, a high-resolution 3D EBSD image of the YSZ coating was obtained.