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The goal of this work was to synthesize refractory §materials like TiN, Ta and alloys of TiN-TaN in the §form of thin films which are used as diffusion §barriers in integrated circuits to prevent diffusion §of Cu into the Si substrate. The primary emphasis§of this research was to synthesize different §microstructures of these films like amorphous,§nanocrystalline, textured polycrystalline and single §crystalline films, and to study the effect of these §microstructures on their mechanical and electrical §properties and on diffusion characteristics of Cu.§Microstructures ranging from nanocrystalline to §single crystalline TiN films on Si(100) substrates §were synthesized by Pulsed Laser Deposition §technique by varying the substrate temperature from §25°C to 650°C. Experimental techniques like XRD, TEM,§HRTEM, STEM-Z, EELS, SIMS and four-point probe §resistivity measurement were used for in-depth §analysis. Effect of microstructures of these films §on their mechanical and electrical properties, and §on diffusion behavior of Cu was analyzed.