A novel approach to measure grain boundary segregation in bulk polycrystalline materials in dependence of the boundaries’ five rotational degrees of freedom

We demonstrate a simplified nondestructive 3-D electron backscatter diffraction (EBSD) methodology that enables the measurement of all five degrees of freedom of grain boundaries (GBs) combined with segregation analysis using atom probe tomography (APT). The approach is based on two 2-D EBSD measurements on orthogonal surfaces at a sharp edge of the specimen followed by site-specific GB composition analysis using APT. An example of an asymmetric Σ9 boundary exhibiting GB segregation emphasizes the need for complete GB characterization in this context.