A facile method to synthesize nanoscale graphene oxide (GO) with controllable interlayer spacing was carried out using two-step oxidation process and much less acid to improve the efficiency of the oxidation. The X-ray diffraction results demonstrated that GO had been successfully prepared from graphite because of disappearance of characteristic peaks of pristine graphite at about 2θ = 26.5 along with appearance of a sharp major peak of GO at about 2θ = 9.4. The increased basal spacing d 001 of as-prepared GO could reach as high as 9.39 Å, suggesting higher degree of oxidation than that prepared by the classical Hummers' synthesis, and characterization results from Fourier transform infrared spectrometer, X-ray photoelectron spectroscopy, Raman spectroscopy, scanning electron microscopy and transmission electron microscopy further confirmed this conclusion. The influence of GO on anti-corrosion performance of nanocomposite coatings composited with the 2,5-dimethoxyaniline (DMA) conductive polymer was examined via potentiodynamic polarization curve tests in 3.5 wt% NaCl aqueous solution. The results demonstrated that the incorporation of GO significantly decreased the corrosion current density (i corr = 2.62 μA/cm 2) in the case of GO-PDMA coating, reflecting excellent physical isolation of GO and its synergistic effect with PDMA against the infiltration of water and corrosive electrolyte.