Ballmilling of In and Sb has been used to produce InSb for use in electroch
emical and in situ X-ray diffraction studies (XRD) of Li/1 M LiPF6 ethylene
carbonate:diethyl carbonate/InSb cells. The cell capacity decays rapidly w
hen cycled between 0 and 1.3 V, while the capacity reduction is less pronou
nced when cycling is restricted to the 0.65-1.4 V range. In situ XRD studie
s reveal that Li3Sb and In are formed during the first plateau (above 0.65
V), according to the reaction 3Li + InSb --> Li3Sb + In. The indium product
subsequently reacts with Li forming the InLix phases InLi and In4Li7 in se
quence. When cells are cycled above 0.6 V (i.e., in the absence of InLix fo
rmation) capacity retention improves significantly, remaining relatively co
nstant near 250 mAh/g. Detailed in situ XRD studies of these cells suggest
that 0.27 Li atoms per InSb may be intercalated during a sharp drop in the
cell potential, according to the reaction xLi + InSb reversible arrow LixIn
Sb (x(max) = 0.27). This intercalation accounts for only a small (about 30
mAh/g) fraction of the overall capacity of 680 mAh/g. Consequently, it appe
ars that the reactivity of In and Sb with Li, not the structure type, deter
mines the reaction path. Therefore, InSb is not an attractive intercalation
host for Li, in contrast to the claims made in the literature. (C) 2001 Th
e Electrochemical Society.