This paper outlines preliminary results from a combined XRD, TEM and APFIM investigation of a rapidly solidified Al 94 V 4 Fe 2 alloy that had been produced by melt spinning. The microstructure produced consists of a high volume fraction (≈50%) of 20 nm icosahedral particles in an f.c.c. matrix. Three-dimensional atom probe analysis shows that this second phase is enriched in iron and vanadium compared with the matrix. The thermal stability of the melt-spun ribbon has been investigated using DSC. It was found to be stable up to a temperature of 520°C, after which there were two solid state transformations.