Conventional sputter deposition techniques produce alternating layers only when Multiple sputtering targets are employed. However, we have demonstrated that the use of only one single Sputtering gun in a conventional sputter deposition process could lead to the formation of alternating layers through self-assembling. The periodicities of the layered structure range from 10degrees to 10(1) nm. The appearance of alternating nano-scaled layers and the periodicity depend on the type of the target materials and the deposition conditions. Based on the consideration of the deposition rate and the catalytic reaction of metal, the Formation such self-assembled alternating nano-scaled layers is explained. (C) 2004 Elsevier B.V. All rights reserved.