The lithiated alloys were synthesized by taking the SbxBi1-x alloys, prepared via melt-spinning, ball milling and annealing, and then ball-milling them with Li metal. To synthesize Li3Bi, a Bi pellet was wrapped in Li foil and fired at 300 °C, because all the material was observed to stick to the milling balls and vial when ball milling was attempted. The powder XRD patterns for the Li3(SbxBi1-x) are shown in Figure . The lattice parameters, grain size and microstrain are summarized in Table . As is the case for the metals, Li3Bi has a larger lattice parameter and unit cell volume than Li3Sb and the peak positions of the intermediate compositions are clearly shifted from Li3Sb towards Li3Bi as the Bi content increases. For all compositions, it appears that a single-phase, face-centered-cubic (fcc) compound can be formed. is that of the material after annealing at 350 °C for 16 hours. As shown in Figure , the as-milled material clearly consists of multiple fcc phases. At higher angles in particular, the peaks are very wide and appear to be composed of at least two separate peaks. Annealing narrows all the peaks considerably, indicative of grain growth, and the peaks of any secondary fcc phases clearly diminish in intensity. As highlighted in the inset of Figure showing the (422) peaks, a small shoulder is still visible on the low-angle side for Li3(Sb0.50Bi0.50), but not for any of the other compositions. The lattice parameter of the secondary phase is close to that of Li3Bi. When attempting to synthesize ternary alloys at a higher temperature (400 °C), disproportionation of the material and segregation of high-temperature (hexagonal) Li3Sb were observed as shown in Figure for Li3(Sb0.25Bi0.75).