Ion beam polishing for three‐dimensional electron backscattered diffraction

Abstract

Summary Serial sectioning by focused ion beam milling for three‐dimensional electron backscatter diffraction (3D‐EBSD) can create surface damage and amorphization in certain materials and consequently reduce the EBSD signal quality. Poor EBSD signal causes longer data acquisition time due to signal averaging and/or poor 3D‐EBSD data quality. In this work a low kV focused ion beam was successfully implemented to automatically polish surfaces during 3D‐EBSD of La‐ and Nb‐doped strontium titanate of volume 12.6 × 12.6 × 3.0 μm. The key to achieving this technique is the combination of a defocused low kV high current ion beam and line scan milling. The line scan was used to restrict polishing to the sample surface and the ion beam was defocused to ensure the beam contacted the complete sample surface. In this study 1 min polishing time per slice increases total acquisition time by approximately 3.3% of normal 3D‐EBSD mapping compared to a significant increase of indexing percentage and pattern quality. The polishing performance in this investigation is discussed, and two potential methods for further improvement are presented.

Is the Ne operation of the helium ion microscope suitable for electron backscatter diffraction sample preparation?

“…A thorough overview of the different EBSD preparation techniques can be found elsewhere [31]. Throughout the past years, Ga-focused ion beam/ scanning electron microscopes (Ga FIB/SEMs) have been used to polish samples [32,33]. Although it is recognized within the FIB community that Ga can induce artefacts in the sample [34][35][36][37], many of the encountered artefacts, which can potentially lead to misinterpretation of the results, are unfortunately never published.…”

3‐D microstructure of olivine in complex geological materials reconstructed by correlative X‐ray ‐CT and EBSD analyses

“…Advances in automated destructive serial-sectioning techniques, including robot-assisted grinding and polishing (Spowart, 2006;Uchic et al, 2012), femtosecond laser ablation (Echlin et al, 2014) or tomography in dual-beam focused ion beam (FIB) microscope (e.g. Zaefferer et al, 2008;West & Thomson, 2009;Saowadee et al, 2013) aim at overcoming these issues for certain applications in materials sciences. In fact, the FIB-assisted 3-D EBSD is a powerful tool in the characterisation of strain, morphology and crystallographic relationships between phases or inclusions, within grains and at grain boundaries (e.g.…”