Focused Ion Beam (FIB) imaging and specimen preparation techniques, and subsequent analysis by either scanning electron microscopy (SEM) in e.g., a DualBeam instrument, or by Transmission Electron Microscopy (TEM) methods, have been utilized successfully for semiconductor, metal, alloy, ceramic, polymer, composite, pharmaceutical, and biological materials. Combining FIB and electron microscopy techniques allows for site specific microstructural characterization, determination of crystallographic information, and elemental composition in either two dimensions, or in 3D via tomographic reconstruction methods, all in the nanometer scale. The advantages of using these combined analytical techniques for the characterization of medical devices materials will be presented. In particular, the microstructural characterization of biological and biocompatible materials such as Nitinol, dental enamel rods, and cell structure will be described.