A new chemical route to prepare the mixed oxide Li 0.7 Ni 0.8 -Co 0.2 O 2 , which is a member of the well-known Li-Ni-Co-O family that is of interest as an electrode material for rechargeable lithium batteries, from a mixed citrate is reported. In a first step the new citrate (NH 4 ) 3 LiNi 0.8 Co 0.2 (C 6 H 5 O 7 ) 2 , is synthesized, which, after thermal decomposition, gives the layered mixed-oxide phase Li 0.7 Ni 0.8 Co 0.2 O 2 . This oxide has been characterized by chemical analysis, XRD, FTIR, SEM, and DTA, revealing an "ideal" trigonal α-NaFeO 2 type struc-