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The formation of a nanocrystalline structure with a grain size of 20-40 nm in the surface layer of amorphous Pd 40 Ni 40 P 20 alloy was observed when crystallization occurred in vacuum. The surface layer was found to be depleted in phosphorus. The nanocrystalline structure with a grain size of 2-20 nm also forms upon crystallization of this amorphous alloy in the electron microscope.