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Recent studies of fcc metals with dense twins (~10 nm spacing) have revealed impressive mechanical properties, along with improved ductility and electrical conductivity in comparison to nanocrystalline metals with similar feature sizes. Many important fcc metals could benefit from these “nanotwinned” microstructures, however, not all fcc metals readily form such twins. The tendency of fcc metals to form twin boundaries is related to the twin boundary energy; those with low twin boundary energy, such as silver (Ag), easily form twins. Increasing twin boundary energy interferes with twin formation, to the point that in metals with high twin boundary energy, like aluminum (Al), twins are quite rare. This thesis focuses on the synthesis of nanotwinned Ag and Al via physical vapor deposition. Nanotwinned Ag is readily fabricated, however, a template approach had to be developed to induce twins in Al. The microstructures and their relationships to observed mechanical properties are also discussed. Grain boundaries interfere with dislocation transmission by posing a slip system discontinuity between grains. Twin boundaries are a special class of grain boundaries in which the grains on either side of the boundary are related by mirror symmetry. Twin boundaries inhibit dislocation transmission, providing strength in the same manner as grain boundaries. However, their symmetrical structure reduces the free volume and grain boundary energy. Accordingly, coherent twin boundaries are often more energetically stable than grain boundaries, and their coherency allows plasticity mechanisms to remain active under conditions where such mechanisms may be inhibited at grain boundaries. Hence, twin boundaries may provide a metal with unique combinations of high strength and good ductility, conductivity, and thermal stability.