Raney-type Ni precursor alloys containing 75 at.% Al and doped with 0, 0.75, 1.5 and 3.0 at.% Ti have been produced by a gas atomization process. The resulting powders have been classified by size fraction with subsequent investigation by powder XRD, SEM and EDX analysis. The undoped powders contain, as expected, the phases Ni 2 Al 3 , NiAl 3 and an Al-eutectic. The Ti-doped powders contain an additional phase with the TiAl 3 DO 22 crystal structure. However, quantitative analysis of the XRD results indicate a far greater fraction of the TiAl 3 phase is present than could be accounted for by a simple mass balance on Ti. This appears to be a (Ti x Ni 1-x )Al 3 phase in which higher cooling rates favour small x (low Ti-site occupancy by Ti atoms). SEM and EDX analysis reveal that virtually all the available Ti is contained within the TiAl 3 phase, with negligible Ti dissolved in either the Ni 2 Al 3 or NiAl 3 phases.