High‐resolution 3D X‐ray diffraction microscopy: 3D mapping of deformed metal microstructures

Three‐dimensional X‐ray diffraction microscopy, 3DXRD, has become an established tool for orientation and strain mapping of bulk polycrystals. However, it is limited to a finite spatial resolution of ∼1.5–3 µm. Presented here is a high‐resolution modality of the technique, HR‐3DXRD, for 3D mapping of submicrometre‐sized crystallites or subgrains with high spatial and angular resolution. Specifically, the method is targeted to visualization of metal microstructures at industrially relevant degrees of plastic deformation. Exploiting intrinsic crystallographic properties of such microstructures, the high resolution is obtained by placing a high‐resolution imaging detector in between the near‐field and far‐field regimes. This configuration enables 3D mapping of deformation microstructure by determining the centre of mass and volume of the subgrains and generating maps by tessellation. The setup is presented, together with a data analysis approach. Full‐scale simulations are used to determine limitations and to demonstrate HR‐3DXRD on realistic phantoms. Misalignments in the setup are shown to cause negligible shifts in the position and orientation of the subgrains. Decreasing the signal‐to‐noise ratio is observed to lead primarily to a loss in the number of determined diffraction spots. Simulations of an α‐Fe sample deformed to a strain of εvM = 0.3 and comprising 828 subgrains show that, despite the high degree of local texture, 772 of the subgrains are retrieved with a spatial accuracy of 0.1 µm and an orientation accuracy of 0.0005°. A full‐field X‐ray diffraction contrast method is presented (high‐resolution 3D X‐ray diffraction), for 3D mapping of plastically deformed microstructures. The essence of the method is the introduction of a 2D detector in the optical mid‐field regime. The properties and limitations of the method are estimated by numerical simulations.