Lithiation was performed at room temperature, as it would be in a battery, by ball milling the powders with a stoichiometric amount of Li foil for 5 hours at 500 rpm on a TenCan XQM-2 planetary mill using 50 ml 304 stainless steel jars and balls. The Sb-Bi starting alloys were processed in 2 g batches using 20 g of balls. Reactants were weighed inside the glovebox on a Mettler Toledo balance with 1 mg readability. Elemental Bi turned out to be too ductile to be milled effectively with Li. To synthesize Li3Bi, a pressed pellet of Bi powder was wrapped in a stoichiometric amount of Li foil and fired on a hotplate set at 300 °C for 16 h in an alumina crucible covered with a quartz glass plate inside an Ar-filled glovebox.