119Sn Mössbauer spectroscopy is used in combination with
7Li MAS NMR spectroscopyand X-ray diffraction to resolve the details of the different Li-Sn and Li-Sb intermetallicsformed during the electrochemical reactions of nominal "SnSb" compounds inside a lithiumbattery. At a Li/SnSb ratio of 2.02, the Mössbauer spectrum indicates that the initial structureof the compounds are not deeply affected during the first steps of discharging. At 4.95 Li/SnSb, each spectrum consists of three components. The hyperfine parameters agree wellwith those of
![](/images/gifchars/beta2.gif)
-Sn and a LiSn-related solid. At 7.27 Li/SnSb, the spectra reveal that nometallic Sn is present. During cell charging, the appearance of a poorly crystalline Li
13Sn
5phase is detected at 8.9 Li/SnSb. NMR data show signals resulting from ionic Li of thepassivating layer and from Li-Sn and Li-Sb intermetallics at downfield and upfield shifts,respectively, which depart from those observed in bulk solids. The partial recovery of thestistaite structure at the end of charging is confirmed in SnSb single-phase electrodes,whereas the opposite is true for mixtures of tin and antimony.