A typical dual-beam platform combines a focused ion beam (FIB) microscope with a field emission gun scanning electron microscope (FEGSEM). Using FIB-FEGSEM, it is possible to sequentially mill away > ~ 50 nm sections of a material by FIB and characterize, at high resolution, the crystallographic features of each new surface by electron backscatter diffraction (EBSD). The successive images can be combined to generate 3D crystallographic maps of the microstructure. A useful technique is described for FIB milling that allows the reliable reconstruction of 3D microstructures using EBSD. This serial sectioning technique was used to investigate the recrystallization behaviour of a particle-containing nickel alloy, which revealed a number of features of the recrystallizing grains that are not clearly evident in 2D EBSD micrographs such as clear evidence of particle stimulated nucleation (PSN) and twin formation and growth during PSN.