Nanoalloys are interesting for several reasons. One of the most exciting features of metal nanoparticles and nanoalloys is that their properties depend on size. This size dependence is related to several phenomena: quantum effects, surface effects, and modifi cation of thermal behavior, among others [ 1 -5 ]. Chemical mixing is another factor that affects the physical and chemical properties of a nanoparticle. Thus the spectrum of possibilities is quite diverse, since the same set of metals A and B may form different structures, depending on the individual elements, thermal conditions, and the synthesis procedure: core-shell nanoparticles [ 6 , 7 ], mixtures, Janus nanoparticles [ 8 ], onion-like nanoparticles (see Fig. 3.1 ) [ 9 , 10 ], or combinations of several of these kinds of structure. If we also include the shape of the particle in the scene, the phase diagram for nanoalloys becomes very rich. To appropriately investigate this phase diagram, a battery of characterization techniques is required.In the last decade, several works have been done in the synthesis of wellcontrolled shape and size-selected metallic and bimetallic nanostructures [ 11 -18 ]. Au-, Pd-, and Pt-based bimetallic nanoparticles were extensively studied since they