The information about the three dimensional (3D) morphology of a material structure is the key to understand the relationships between its manufacturing parameters and its properties. Moreover, its crystallographic and chemical information become also unavoidably necessary if the processing and the properties of materials has to be optimized for a specific application. Dual Beam workstations combining a Focused Ion Beam (FIB) with Scanning Electron Microscopy (SEM) have shown to be a very versatile tool for studying the microstructure with different possibilities, like for instance cross sectioning, tomography, site-specific preparation of thin foils, or FIB-imaging [1]. The outstanding capabilities of the FIB technique can be further expanded when combined with alternative techniques, as for instance Electron Backscattered Diffraction (EBSD). On one side, FIB polishing provides an optimal surface quality for EBSD, and therefore can be used for the preparation of samples, including also the realization of FIB/EBSD tomographies. On the other side, thin films can be prepared by FIB and analyzed in transmission with EBSD (also known as Transmission Kikuchi Diffraction [2]).

In this work we will present different advanced characterization possibilities (tomography, TKD, site-specific preparation) applied to the study of metal matrix nanocomposites, including Ni reinforced with carbon nanotubes, onion-like carbons and nanodiamonds. These nanoparticles have already shown the capability of tailoring the microstructure and stabilizing it against thermal loading [3, 4]. Thereby, the study of this model material by the aforementioned complementary techniques will allow us to understand (with a high grade of accuracy) the microstructural evolution under mechanical stresses, particularly in tribological applications.