ACOM/TEM and EBSD Microstructure Characterization of ECAE-Processed Zirconium

Materials produced through equal channel angular extrusion (ECAE) may offer enhanced mechanical properties over classic thermomechanical processing like extrusion or rolling. Conventional techniques such as electron backscatter diffraction (EBSD) may be insufficient to properly characterize the microstructure of these materials. Darkfield (DF) transmission electron microscopy (TEM), on the other hand, may lead to erroneous conclusions with respect to grain size. In this work, zirconium was submitted to ECAE deformation through four passes in the Bc route at 350 °C. The microstructure was evaluated through FEG-SEM/EBSD (field emission gun–scanning electron microscopy), DF TEM, and ACOM/TEM (automated crystal orientation mapping in TEM). EBSD revealed that the microstructure was heterogeneous with a few large grains surrounded by a fine submicrometric structure, which was only partially resolved through this technique. The fine structure was, however, described through ACOM/TEM. DF TEM was revealed to be somewhat unreliable when the same region was evaluated through ACOM/TEM. Therefore, a combination of techniques seems to be required for proper characterization.