Congruently melting, single-phase Ni 5 Ge 3 (T m = 1185°C) has been rapidly solidified via drop-tube processing wherein powders, with diameters between 850 -53 m, are produced. At low cooling rates (850 -150 m diameter particles, 700 -7800 K s -1 ) the dominant solidification morphology, revealed after etching, is that of isolated plate & lath microstructure in an otherwise featureless matrix. At higher cooling rates (150 -53 m diameter particles, 7800 -42000 K s -1 ) the dominant solidification morphology is that of isolated faceted hexagonal crystallites, again imbedded within a featureless matrix. Selected area diffraction analysis in the TEM reveals the plate & lath, and isolated hexagonal crystallites, are a disordered variant of -Ni 5 Ge 3 , whilst the featureless matrix is the ordered variant of the same compound. Thermal analysis and in situ heating in the TEM indicate a reversible solid-state order-disorder transformation between 470 -485°C.