This paper discusses the ex situ preparation of Li nanocomposite materials for use as Li battery anodes. The syntheses involve high-temperature, hydrogen-driven, solid-state reactions consisting of alloy disproportionation and metathetical transformations. The following systems are described, LiAlH4/SnO, LiAlH4/SiO2, and LiH/SnO, as well as pertinent electrochemical properties of their nanocomposite products. The properties of nanoscale LiAl particles produced by the decomposition and subsequent disproportionation of LiAlH4 are also discussed. Electrochemical experiments were carried out using Li metal as the anode. The possible extension of the process to appropriate, precursor intermetallic compounds is also examined.