The electrochemical reduction of metal oxides provides an appropriate techn
ique for the production of nanocrystalline mesoporous metals at room-temper
ature. Polycrystalline sintered CuO and Cu2O single crystals were reduced t
o Cu in this study. Electron microscopy and diffraction results demonstrate
the dependence of the metal microstructure on the preparation and post-tre
atment conditions. The size and microstrain of the crystallites are control
led mainly by the preparation temperature. This method enables the reproduc
ible production of medium-scale nanocrystalline metals independent on criti
cal process parameters. (C) 2000 Kluwer Academic Publishers.