SummaryThis study investigates the effect of focused ion beam (FIB) current and accelerating voltage on electron backscatter diffraction pattern quality of yttria-stabilized zirconia (YSZ) and Nb-doped strontium titanate (STN) to optimize data quality and acquisition time for 3D-EBSD experiments by FIB serial sectioning. Band contrast and band slope were used to describe the pattern quality. The FIB probe currents investigated ranged from 100 to 5000 pA and the accelerating voltage was either 30 or 5 kV. The results show that 30 kV FIB milling induced a significant reduction of the pattern quality of STN samples compared to a mechanically polished surface but yielded a high pattern quality on YSZ. The difference between STN and YSZ pattern quality is thought to be caused by difference in the degree of ion damage as their backscatter coefficients and ion penetration depths are virtually identical. Reducing the FIB probe current from 5000to 100 pA improved the pattern quality by 20% for STN but only showed a marginal improvement for YSZ. On STN, a conductive coating can help to improve the pattern quality and 5 kV polishing can lead to a 100% improvement of the pattern quality relatively to 30 kV FIB milling. For 3D-EBSD experiments of a material such as STN, it is recommended to combine a high kV FIB milling and low kV polishing for each slice in order to optimize the data quality and acquisition time.

Kikuchi bands in election backscattered diffraction patterns (EBSP) contain information about lattice constants of crystallographic samples that can be extracted via the Bragg equation. An advantage of lattice constant measurement from EBSPs over diffraction (XRD) is the ability to perform local analysis. In this study, lattice constants of cubic STN and cubic YSZ in the pure materials and in co-sintered composites were measured from their EBSPs acquired at 10 kV using a silicon single crystal as a calibration reference. The EBSP distortion was corrected by spherical back projection and Kikuchi band analysis was made using in-house software. The error of the lattice constant measurement was determined to be in the range of 0.09-1.12% compared to values determined by XRD and from literature. The confidence level of the method is indicated by the standard deviation of the measurement, which is approximately 0.04 Å. Studying Kikuchi band size dependence of the measurement precision shows that the measurement error decays with increasing band size (i.e. decreasing lattice constant). However, in practice, the sharpness of wide bands tends to be low due to their low intensity, thus limiting the measurement precision. Possible methods to improve measurement precision are suggested.

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.