In situ transmission Kikuchi diffraction tensile testing

We present a methodology for in situ Transmission Kikuchi Diffraction (TKD) tensile testing that enables nanoscale characterization of the evolution of complex plasticity mechanisms. By integrating a modified in situ scanning electron microscope nanoindenter with a microscale push-to-pull device and a conventional Electron Backscatter Diffraction (EBSD) detector, we achieved TKD measurements at high spatial resolution during mechanical deformation. A dedicated focused ion beam procedure was developed for site-specific specimen fabrication, including lift-out, thinning, and shaping into a dog-bone geometry. The methodology was demonstrated on two case studies: (i) a metastable β-Ti single crystal, on which we quantified the initiation and evolution of nanoscale twinning and stress-induced martensitic transformation, and (ii) a CuAl/Al₂O₃ nanolaminate, which showed nanoscale plasticity and twinning/detwinning in a complex microstructure. Overall, this approach provides a robust alternative to in situ EBSD and transmission electron microscopy testing, facilitating detailed analysis of deformation mechanisms at the nanoscale.