A Scanning Electron Microscope (SEM) equipped with a Focused Ion Beam (FIB) was used to analyze the gamma-gamma'-microstructure of a Ni-based superalloy in 3D. Serial sectioning was combined with imaging by a Circular BackScatter (CBS) detector resulting in an angular ablation of the sample. Postprocessing of the image series applying tilt corrections and slice alignment operations resulted in a properly aligned volume with high resolution and little noise. Evaluation of the 3D microstructural data will be presented. The results can be used to estimate the reliability of microstructural data obtained from 3D stereographic reconstructions from 2D images.