With proper sample preparation, high temperature x-ray diffraction can be used to study in-situ the reactions occurring at a solder/metal interface. We have applied this technique to an investigation of the reaction kinetics between copper and nickel metal and 60/40 Sn/Pb solder. The copper and nickel are shown to follow similar pathways, each having a complex reaction profile that involves an initial “hold” of little reactivity, followed by a two-step diffusion controlled reaction. Activation energies were obtained from Arrhenius-type plots, and result in values of 6.8 kcal/mole for the nickel/solder reaction, and 13 kcal/mole for the copper/solder reaction. These results are compared with those obtained by previous investigators, and discussed in terms of the growth of the different intermetallic phases.