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From X‐ray studies of iron‐nickel‐aluminium alloys a new phase a′ was discovered. Although, in the surface layers of these alloys an unstable γ‐phase is observed in the early stage of annealing, this phase disappears entirely with prolonged annealing, the X‐ray pattern showing the co‐existence of the a‐ and a′‐phases. In the interiors of the specimens the unstable γ‐phase is never found, only diffused X‐ray interference lines being observed there. However, by very long annealing extending to 3,500 hours at 1,000 deg., the writer succeeded in observing a splitting phenomenon of the X‐ray pattern in the interiors of the specimens also.