The electrochemical reaction mechanisms between lithium and cystalline MnSb are investigated by X-ray diffraction, 121Sb Mössbauer spectroscopy, and X-ray absorption spectroscopy (XAS). The analysis of the experimental data at different depths of the electrochemical discharge process reveals a complex reaction mechanism comprising two steps. The main reaction of the first step corresponds to the dispersion of lithium in the MnSb matrix with formation of the intermediate compound LiMnSb. The second step corresponds to a Li–Sb alloying process with formation of Li3Sb.
