Nondestructive three-dimensional mapping of grain shape, crystallographic orientation, and grain boundary geometry by diffraction contrast tomography (DCT) provides opportunities for the study of the interaction between intergranular stress corrosion cracking and microstructure. A stress corrosion crack was grown through a volume of sensitized austenitic stainless steel mapped with DCT and observed in situ by synchrotron tomography. Several sensitization-resistant crack-bridging boundaries were identified, and although they have special geometric properties, they are not the twin variant boundaries usually maximized during grain boundary engineering.
Increasingly researchers are looking to bring together perspectives across multiple scales, or to combine insights from different techniques, for the same region of interest. To this end, correlative microscopy has already yielded substantial new insights in two dimensions (2D). Here we develop correlative tomography where the correlative task is somewhat more challenging because the volume of interest is typically hidden beneath the sample surface. We have threaded together x-ray computed tomography, serial section FIB-SEM tomography, electron backscatter diffraction and finally TEM elemental analysis all for the same 3D region. This has allowed observation of the competition between pitting corrosion and intergranular corrosion at multiple scales revealing the structural hierarchy, crystallography and chemistry of veiled corrosion pits in stainless steel. With automated correlative workflows and co-visualization of the multi-scale or multi-modal datasets the technique promises to provide insights across biological, geological and materials science that are impossible using either individual or multiple uncorrelated techniques.
Intergranular stress corrosion cracking in a sensitised type 302 stainless steel wire has been observed in situ using high resolution X-ray microtomography. Tomography enables the development and failure of crack bridging ligaments to be studied in detail in three dimensions. Direct comparison of these features has been made with scanning electron microscopy fractography. The crack bridges failed in a ductile manner, with a morphology that is consistent with non-sensitised low energy grain boundaries.