Electron Backscatter Diffraction (EBSD) has been used in conjunction with a Scanning Electron Microscope (SEM) combined with a focused ion beam (FIB) instrument to obtain three dimensional (3D) high resolution characterizations of crystalline microstructures. This work reports on continued development that has proceeded on this technique. The technique is based on automated in-situ serial sectioning using the FIB and characterization of the sections using automated EBSD or orientation imaging microscopy (OIM). The technique extends the powerful features of two dimensional OIM into the third spatial dimension. This allows additional descriptive microstructural parameters to be obtained, for example the morphology and the crystallographic indices of interface planes. This paper provides an overview of the technique and shows results from two different samples: pearlite colonies in a high carbon steel and twin related grain triplets in a NiCo thin film.