The fabrication of bilayer and multilayer Mo/Al thin films using a conventional multi-target rf-diode sputter deposition system was studied. The films were deposited on glass and Si( 100) substrates. The as-deposited films were characterized with respect to their structure and composition profiles using X-Ray diffraction, AES, SEM, TEM, and RBS techniques. The as-deposited bilayer films were of good quality with an interface thickness of about 200 Ã . They were annealed at different temperatures in the range of 300-600°C for different times. Diffusional intermixing and phase changes were monitored and diffusivity measurements were made. The growth characteristics of intermetallic compounds were analysed. Mo/Al multilayer thin films with layer thicknesses less than 200 Ã were also deposited. An assessment of structural and compositional modulations in these multilayer films revealed the need for the conversion of the conventional diode sources to magnetron sources for improvement of film quality. Also presented are a few preliminary theoretical calculations for high-energy ion-beam mixing of the Mo/Al bilayer thin films. / Master of Science