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High Quality Sample Preparation for EBSD Analysis by Broad Ion Beam Milling

Electron Backscatter Diffraction technique (EBSD) is known as a "surface" technique because electron diffraction is generated within a few tens of nanometers of the sample surface. Therefore, the specimen surface should be exempt of any damages in order to produce EBSD patterns. Here, we present a successful and efficient EBSD sample polishing of two very challenging specimens prepared by broad ion beam milling.

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Method: Cross sectioning by ion beam slope cutting

Fig. 1: a) At first, a mechanical pre-preparation is performed using the Leica TXP (cross sectioning) to approach the area of interest in a very short time. b) Then, with the Leica TIC 3X (broad ion milling) a perfect cross-section surface is achieved, which is ready for EBSD analysis.

Results on a semiconductor

Results on a aluminum/diamond/graphite composite

Fig. 3c: EBSD patterns of the different phases.

SE image

Fig. 3d: Overview of the prepared surface (in total 3 mm were polished).

Pattern quality map

Fig. 3e: Pattern quality map of the EBSD/EDS analysis.

EBSD phase map

Fig. 3f: EBSD Phase map showing the high indexing rate, even on the graphite flakes. Graphite is displayed in blue, diamond in red and aluminum in green.

IPF X map

Fig. 3g: Corresponding EBSD orientation map along the X axis.

Conclusions

While the Focused Ion Beam technique is often used for site specific sample preparation, it usually prevents from a successful EBSD analysis by introducing sub-surface deformation and curtaining especially on multiphase material. In this example we have demonstrated that broad ion beam milling allows to simultaneously polish both hard and soft material.

The combined use of the Leica EM TXP and the Leica EM TIC 3X allows to perfectly prepare large areas of very challenging samples within a short time.

Acknowledgement

We thank Andi Kaeppel and Roald Tagle for taking the M4 picture, Figure 2b.

Reference

Gang Ji, et al.: Materials Characterization 89: 132–37 (2014).