Plan-view sample preparation of a buried nanodots array by FIB with accurate EDS positioning in thickness direction

Abstract

Recently, there are growing demands on focus ion beam (FIB) sample preparation technique in plan-view geometry because it can provide the in-plane microstructure information of thin film and allows direct correlations of the atomic structure via transmission electron microscopy with micrometer-scale property measurements. However, one main technical difficulty is to position the buried thin film accurately in a sandwich structure. In this paper, an on-line positioning method based on the thickness monitoring by EDS is introduced, where the intensities of the characteristic X-ray peaks from different layers are proportional to the relative thickness of them at the same acquisition conditions. A high density array of ∼100 nm squares BiFeO3 nanodots with ∼ 25 nm thickness grown on a 20 nm thick SrRuO3 bottom electrode and (001)-oriented SrTiO3 substrate is selected for demonstration. By monitoring the intensities of Pt-M, Sr-L, Ti-K, Ru-L, Fe-K and Bi-M peaks, the relative thickness of Pt protection layer, the BiFeO3, SrRuO3 and SrTiO3 can be obtained, which provide accurate position of the BFO nanodots array in the thickness direction. With these information, the cutting parameters are optimized and a high quality plan-view specimen of BFO nanodots array is prepared, which is confirmed by high resolution transmission electron microscopy. This positioning method should have a wide application for material science.