This thesis is devoted to the deposition of intermetallic thin films by laser ablation deposition (LAD) and their characterization. Pulsed laser ablation and subsequent deposition of the ablated vapours produces films under conditions very far away from equilibrium. Besides the film, which forms directly by quenching the vapour or plasma on substrate, one also obtains under certain conditions micron and sub-micron sized spherical droplets of alloy melt on to the film. The latter travel at very high velocities and impinge on the substrate resulting in a very high rate of heat transfer during solidification from liquid state. Therefore, in this work it was possible to study the microstructure evolution depending on quenching rates of different sized droplets and compare with the extreme case of vapour/plasma quenching. The compositions selected correspond to the intermetallic compounds in Al-Fe, Al-Ni and Ti-Si binary systems. Pre-alloyed targets of the appropriate intermetallic compositions were used for ablation by laser. The deposition system has been designed and built in-house. The characterization is mainly done by transmission electron microscopy (TEM). The study focuses on microstructure and phase evolution within these intermetallic films at room temperature, at elevated temperature and during heating the room temperature deposited films in heating stage inside the TEM.