The short-range order (SRO) structure of a Au-25 at. pct Fe single crystal was studied using wide-angle diffuse synchrotron X-radiation scattering at room temperature. Two heat treatments were investigated: a 400 °C aging treatment for 2 days and a 440 °C treatment for 5 days, both preceded by solution treatment in the single-phase field and water-quenched to room temperature. Evolution of the SRO structure with aging was determined by fitting the two sets of Cowley-Warren (C-W) SRO parameters to a pair of 140,608-atom models. The microstructures, although quite disordered, showed a trend with aging for an increasing volume fraction of an Fe-enriched and an Fe-depleted environment. The Fe-enriched environment displayed a preference for Fe segregation to the {110} and {100} face-centered cubic (fcc) matrix planes. A major portion of the Fe-depleted environment was found to contain elements (and variations of these elements) of the Dl ordered superstructure. The SRO contained in the Fe-depleted environment may be best described in terms of the standing concentration wave packet (SCWP) model. This study provides, for the first time, a quantitative real-space view of the atomic arrangements, which make up both environments in the SRO structure of Au-25 at. pct Fe. © 1994 The Minerals, Metals and Materials Society, and ASM International.