A stable hydrosol of graphene was synthesized by oxidation reduction and then a flow assembly of this graphene was used to form a graphene-based membrane by vacuum extraction filtering method. X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy, particle size analysis, and scanning probe microscopy (SPM) were used to characterize the crystal structure, granularity, and characteristic change of the molecular spectrum of the samples in the reaction. FTIR tests show that the structural layer of graphite during the oxidation process bonds to a large number of functional groups and parts of these stable functional groups remain on the reduced structural layer of graphene. X-ray diffraction results show that the peaks of the graphite oxide shift to lower angles, become broader and the original graphite peak disappears. Suspensions of graphene oxide form condensed matter and graphene flocculating constituent during film deposition. Particle size analysis and SPM tests show that the particle sizes of the graphene oxide sheets that are dispersed in water show a tailing peak and a broad distribution while the graphene sheets show a singlet, narrower distribution, and smaller dimensions. Raman results show that during oxidation and reduction, the D peak and G peak of the samples gradually extend, ID/IG increases gradually and the degree of sample disorder increases. On the basis of the above analyses, the structural characteristics of the samples in the reaction are summarized.