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Summary Preparation of specimens for electron backscatter diffraction has to be done with great care to ensure a high indexing fraction from high‐quality patterns. Despite the amount of published and recommended preparation methods for different materials, detailed information about the preparation parameters are either missing, or different preparation methods are recommended for one material. The aim of this contribution is to compare the application of several preparation techniques on different metallic samples to determine a suitable preparation method for high‐quality electron backscatter diffraction measurements for a variety of alloys. From the results obtained, polishing with an oxide polishing suspension is the most appropriate preparation method for the materials and preparation methods investigated. Furthermore, the influence of mechanical polishing as well as of oxide polishing suspension polishing on misorientation is found to be negligible for misorientation angles greater than 1°. In the course of this study the absolute indexing reproducibility of the EBSD‐system employed was determined to be 1.18° with respect to the misorientation angle θ.

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