We propose a novel technique for the large-scale synthesis of aligned-plate nanostructures that are self-assembled and self-supporting. The synthesis technique involves developing nanoscale two-phase microstructures through discontinuous precipitation followed by selective etching to remove one of the phases. The method may be applied to any alloy system in which the discontinuous precipitation transformation goes to completion. The resulting structure may have many applications in catalysis, filtering and thermal management depending on the phase selection and added functionality through chemical reaction with the retained phase. The synthesis technique is demonstrated using the discontinuous precipitation of a γ' phase, (Ni, Co)3Al, followed by selective dissolution of the γ matrix phase. The production of the nanostructure requires heat treatments on the order of minutes and can be performed on a large scale making this synthesis technique of great economic potential.