This chapter investigates microstructural features in three dimensions. The study focuses on an additively manufactured (AM) nickel alloy with ultrafine grains as the base material. Sample preparation and characterization were performed using a dual-beam electron microscope equipped with focus ion beam milling (FIB). A specific area of the base material was selected, sectioned using the FIB column, and a micro-sized chunk box was extracted. This chunk box underwent a characterization cycle involving repetitive electron backscatter diffraction (EBSD) pattern detection and FIB milling. Subsequently, layer-by-layer EBSD data from the chunk box were assembled to construct a 3D representation of the microstructure. The layer-by-layer EBSD data of the chunk box was then assembled, resulting in a 3D representation of the microstructure that includes volumetric grain information. This innovative technique facilitates a more comprehensive study of additive manufacturing materials compared to conventional 2D methods.