Nanoparticles of lithium cobalt oxide (LiCoO2) and nanosheets of lithium vanadium oxide (LiV3O8) were synthesized by a citrate sol–gel combustion route. The physical characterizations of the electrodic materials were carried out by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and also X-ray diffraction (XRD) measurements. Near spherical nanoparticles of ≈100 nm and compact nanosheets with a few nanometers thick were observed by SEM and TEM for LiCoO2 and LiV3O8, respectively. XRD data indicated that the as-prepared active materials presented pure phase of rhombohedral LiCoO2 with R-3m symmetry and monoclinic LiV3O8 with p21/m symmetry. The kinetics of electrochemical intercalation of lithium ion into the nanoparticles of LiCoO2 and nanosheets of LiV3O8 from 1.0 mol l−1 LiNO3 aqueous solution were investigated by cyclic voltammetry and chronoamperometry. An aqueous rechargeable lithium-ion battery consisting of LiCoO2 nanoparticles as positive and LiV3O8 nanosheets as negative electrode was assembled. This battery represented a discharge voltage of about 1 V with good cycling performance.