Ternary Ni-based amorphous films can serve as a barrier layer for Cu interconnects in ultralarge-scale integration (ULSI) applications. In this paper, Ni-Mo-P films deposited on silicon wafers without a complicated pretreatment such as Pd activation were prepared using a nonisothermal deposition (NITD) method. The deposition solutions and operating conditions for preparing the Ni-Mo-P alloys are presented, and the effect of the concentration of MoO42- added in electrolytes on the deposition rate is investigated. The surface morphology, microstructures, compositions, and electrical resistivity of the Ni-Mo-P deposits are also thoroughly examined. Based on the experimental results, the Ni-based ternary alloys produced by the NITD method contain high levels of both Mo and P, and the properties of Ni-Mo-P films are dependent on the concentration of molybdate in electrolytes. It is concluded that the Ni-Mo-P thin films produced by the proposed approach in this study are promising for the 60 nm technologies in ULSI. (C) 2008 The Electrochemical Society.