Several techniques have been investigated for making alloy libraries for combinatorial materials development. In this investigation, we demonstrate a method for Ni-Fe-Cr ternary alloy library preparation by deposition of three layers of different metals with a linear thickness gradient rotated by 120degrees for each layer. The layers were interdiffused and alloyed by annealing in vacuum. The resulting specimens were analyzed and compared with the well-known phase diagram for this system by means of rapid x-ray diffraction mapping with synchrotron radiation. (C) 2004 American Vacuum Society.