In this thesis, a comprehensive investigation is conducted into the solid-state reaction between cobalt-disilicide (Co2Si) and solid zinc (Zn), with particular focus on the formation of periodic layered microstructures. The interaction between Co2Si and Zn is examined at 390°C, and samples are annealed for various durations to study the development of alternating layers. The reaction zone is characterised using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM). Additionally, 3D imaging and analytical mapping are presented to provide a detailed visualisation of the reaction dynamics.