Nanoscale energy storage materials offer enhanced kinetics, material stability and gravimetric capacity, with respect to their bulk counterparts. Hydrogen‐driven metallurgical reactions (HDMR) represent a novel method for synthesis of these nanomaterials. Nanoscale and nanocomposite electrodes for Li‐ion batteries synthesized by HDMR demonstrate reversible lithium cycling at low temperature (298 °C). The nanocomposite electrodes are composed of an electrochemically active species (Li‐Sn, Li‐Al‐Sn and Li‐Al‐Si) imbedded within an inert Li2O matrix. These electrodes are prepared in the charged state and therefore do not suffer from the first cycle capacity loss that is characteristic of the intermetallic anodes. This novel synthesis technique may also be applied to the preparation of new hydrogen storage compounds.