The decomposition rates of Ni(PF 3 ) 4 and Pt(PF 3 ) 4 on the growing surface, which are useful for Pt-Ni alloy thin film deposition, were studied by using the macro cavity analysis. The activation energies for these gasdecomposition were obtained 1.0 and 0.86eV, respectively. The Pt source requires the smaller thermal energy. Therefore, it is suggested that when the Pt-Ni alloy film at the high temperatures, the Pt/Ni ratio of the film deposited in the trench will swiftly decrease as increasing the distance from the open area, as well as the trench quality decreases.