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 ε vM = 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°.

In situ visualization of long-range defect interactions at the edge of melting.

Connecting a bulk material's microscopic defects to its macroscopic properties is an age-old problem in materials science. Long-range interactions between dislocations (line defects) are known to play a key role in how materials deform or melt, but we lack the tools to connect these dynamics to the macroscopic properties. We introduce time-resolved dark-field x-ray microscopy to directly visualize how dislocations move and interact over hundreds of micrometers deep inside bulk aluminum. With real-time movies, we reveal the thermally activated motion and interactions of dislocations that comprise a boundary and show how weakened binding forces destabilize the structure at 99% of the melting temperature. Connecting dynamics of the microstructure to its stability, we provide important opportunities to guide and validate multiscale models that are yet untested.

Imaging microstructural dynamics and strain fields in electro-active materials in situ with dark field x-ray microscopy.

The electric-field-induced and temperature induced dynamics of domains, defects, and phases play an important role in determining the macroscopic functional response of ferroelectric and piezoelectric materials. However, distinguishing and quantifying these phenomena remains a persistent challenge that inhibits our understanding of the fundamental structure-property relationships. In situ dark field x-ray microscopy is a new experimental technique for the real space mapping of lattice strain and orientation in bulk materials. In this paper, we describe an apparatus and methodology for conducting in situ studies of thermally and electrically induced structural dynamics and demonstrate their use on ferroelectric BaTiO3 single crystals. The stable temperature and electric field apparatus enables simultaneous control of electric fields up to ≈2 kV/mm at temperatures up to 200 °C with a stability of ΔT = ±0.01 K and a ramp rate of up to 0.5 K/min. This capability facilitates studies of critical phenomena, such as phase transitions, which we observe via the microstructural change occurring during the electric-field-induced cubic to tetragonal phase transition in BaTiO3 at its Curie temperature. With such systematic control, we show how the growth of the polar phase front and its associated ferroelastic domains fall along unexpected directions and, after several cycles of electric field application, result in a non-reversible lattice strain at the electrode-crystal interface. These capabilities pave the way for new insights into the temperature and electric field dependent electromechanical transitions and the critical influence of subtle defects and interfaces.