Magnetostrictive Fe 100−x Ga x alloys over the composition range 0 < x < 36 have been prepared by combinatorial sputtering methods. These films were investigated by x-ray diffraction and 57 Fe Mössbauer effect spectroscopy techniques that have been adapted for the efficient study of combinatorial samples. X-ray diffraction measurements show the presence of a disordered bcc phase with a lattice parameter that increases with increasing Ga content. Mössbauer effect measurements show that even for low Ga content the disordered alloys are not truly random but show some degree of short range Ga clustering. For x > 20, the Mössbauer effect results suggest the presence of short range D0 3 type order. This persists up to the maximum Ga content studied here (x = 36), although there is no evidence to support the formation of long range D0 3 structural order in any of the films prepared in this study.