The electrical, chemical, and structural interactions between Ni films and In 0.53 Ga 0.47 As for source-drain applications in transistor structures have been investigated. It was found that for thick (> 10 nm) Ni films, a steady decrease in sheet resistance occurs with increasing anneal temperatures, however, this trend reverses at 450°C for 5 nm thick Ni layers, primarily due to the agglomeration or phase separation of the Ni-(In,Ga) As layer. A combined hard-x-ray photoelectron spectroscopy (HAXPES) and x-ray absorption spectroscopy (XAS) analysis of the chemical structure of the Ni-(In,Ga)As alloy system shows: (1) that Ni readily interacts with In 0.53 Ga 0.47 As upon deposition at room temperature resulting in significant interdiffusion and the formation of NiIn, NiGa, and NiAs alloys, and (2) the steady diffusion of Ga through the Ni layer with annealing, resulting in the formation of a Ga 2 O 3 film at the surface. The need for the combined application of HAXPES and XAS measurements to fully determine chemical speciation and sample structure is highlighted and this approach is used to develop a structural and chemical compositional model of the Ni-(In,Ga)As system as it evolves over a thermal annealing range of 250 to 500°C.