▎ 摘　　要

In this work, single-layer layered double hydroxide (LDH) nanosheets were prepared by exfoliation of highly crystalline Co-Al-NO3 LDH. Graphene oxide (GO) nanosheets were prepared by the exfoliation of natural graphite oxides in water. By utilizing the hydrogen-bonding layer-by-layer self-assembly method, poly(vinyl alcohol) (PVA) hybrid films with highly oriented GO and LDH were fabricated. By a simple and effective in situ reduction process, multilayer nanocomposite films containing monolayer dispersed graphene and LDHs can be obtained. It was Found that the pi-conjugation network within the graphene nanosheets was gradually recovered during the reduction process and a critical time for the formation of conductive paths for electron transfer was obtained. The relatively complete reduced hybrid film exhibited significantly improved electrical conductivity compared with the unreduced one. These heterogeneous composite films with monolayer dispersed and aligned graphene and LDHs are expected to find potential applications in electrodes and multifunctional nanocomposites.