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Large area polystyrene spheres (PS) arrays with different diameters were prepared by an interface self-assembly method.The self-assembled PS arrays were hexagonal and close-packed, the inter-particle spacing of PS arrays was adjusted by O2-plasma treatment.When O2-plasma treatment time reached 120 s, the space of PS arrays increased to 80~88 nm.After electron beam deposition of gold, and the removing the PS masks by dissolution in dichlommethane with the aid of sonication,we can fabricate the metal micro-nano holes arrays with different diameter.