The Sb-Bi solid solutions with compositions Sb0.25Bi0.75, Sb0.50Bi0.50 and Sb0.75Bi0.25 were prepared as starting materials by melt spinning followed by annealing. Melt spinning was performed on an Edmund Buehler GMBH SC10 single-roller melt spinner. Compacted powder pellets of the desired overall composition were loaded into a BN crucible and induction melted using a 5 kW HU5 RF generator. The melting process was monitored using a pyrometer. The melt was ejected at a temperature of 700 750 °C onto a 30 cm diameter copper wheel spinning at 40 Hz, corresponding to a surface velocity of 38 m/s. The resulting materials were not yet singlephase and were crushed in an agate mortar, milled for 30 minutes using 304 stainless steel milling tools at 500 rpm and annealed on a hotplate. The annealing temperature was set to the solidus temperature for that particular composition, ranging from 300 °C for Sb0.25Bi0.75 to 380 °C for Sb0.75Bi0.25, for 16 hours, under argon.