The development of structural and functional materials has decisively and sustainably influenced the evolution of mankind. Whereas the internal structure of engineering materials and material systems was relatively simple a few decades ago, their microstructure has since become much more complex, and the constituents that control their properties have become smaller and smaller. Furthermore, the microstructure is determined by the manufacturing technology, as, for example, in additive manufacturing. The presentation deals with the development and characterization of high-performance materials, ranging from the complex structure of intermetallic titanium aluminides to the analysis of grain boundaries in molybdenum. For the metallographic investigations, cross-scale techniques were employed, which bridge the gap between the macrostructure and the atomic structure. In order to acquire a complete understanding of the materials based on their comprehensive characterization, complementary methods such as diffraction and scattering with neutrons and synchrotron radiation as well as nanoindentation were adopted.