Focused Ion Beam Parameters for the Preparation of Oxidic Ceramic Materials

Abstract

The interaction of a Ga+ focused ion beam (FIB) with oxidic materials (mullite, alumina, titania, MgO‐partially stabilized ZrO2 (Mg‐PSZ), Y2O3‐partially stabilized ZrO2 (Y‐PSZ), MgO) is investigated to identify suitable parameters for sample preparation for surface‐sensitive analytical methods, e.g., electron backscatter diffraction (EBSD) by varying the parameters glancing angle and applied power. The statistical analysis shows that the influence of the FIB parameters on the surface quality corresponds well to the literature. The data yield that mild parameter levels reduce the surface damage and should be used for final preparation steps of oxides. Furthermore, correlations between the theoretical damage depth and observed EBSD data are only partly confirmed and other properties are relevant to understanding the materials' behavior. For Al2O3 and MgO, the theoretical damaging behavior corresponds well to the observed data. Mullite shows similar properties to alumina and magnesia and deviations are related to a possibly strong Ga+ implantation. Zirconia and titania interact strongly with the ion beam. ZrO2 shows a phase transformation due to heating and the stabilization of high‐temperature phases because of gallium oxide implantation. For TiO2, a strong surface amorphization is registered, which is related to preferential sputtering of oxygen and the existence of various oxidation states.