The ability to obtain three-dimensional information has always been important to gain insight and understanding into material systems. Three-dimensional reconstruction often reveals information about the morphology and composition of a system that can otherwise be obscured or misinterpreted by two-dimensional images. In this article, we describe tomographic measurements with 10 nm scale resolution, combining focused ion-beam processing with field-emission scanning electron microscopy to obtain a series of high-resolution two-dimensional cross-sectional images. The images were then concatenated in a computer and interpolated into three-dimensional space to assess and visualize the structure of the material. The results of this research demonstrate the use of tomographic reconstruction of Si-Si/Ge and theta' Al2CU samples to reproduce the three-dimensional morphology with sub-10 nm resolution. (c) 2006 American Vacuum Society.