Thin film couples of gold/tin are prepared at room temperature under high vacuum conditions by sequential evaporation of high purity metals. Different sets of couples are prepared by changing the sequence of deposition of the metal films. Couples of gold and tin films with offset configuration are prepared also. The couples are annealed at different temperatures for different periods of time to study the interdiffusion between the metal films. The structure of the as-deposited and annealed samples is investigated by transmission electron microscope. Various phases formed in the couples are identified by electron diffraction technique.