New graphitic carbon nitride (g-C3N4) supercell structures, including microsheets, nanorods and microprisms were prepared via the two-step method of the calcination and hydrothermal post-treatment, in which the concentrations of bulk g-C3N4 precursors were controlled before the hydrothermal treatment. After hydrothermal treatment of 20, 100, 200 mg mL(-1) bulk g-C3N4 precursor, the hexagonal unit cell parameters of asprepared g-C3N4 supercell structures are: a = b = 16.46 angstrom, c = 6.49 angstrom, alpha = beta = 90 degrees, gamma = 120 degrees. The crystallographic structures, morphologies, optical and chemical properties of g-C3N4 samples were characterized by Xray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscope (TEM), electron diffraction (ED), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR), N2 adsorption/desorption isotherms, photoluminescence (PL) spectroscopy, and UV-vis diffuse reflectance spectroscopy (DRS). Photocatalytic performances of the g-C3N4 samples were evaluated by the degradation of Rhodamine B in an aqueous medium under visible-light irradiation. Photodegradation activity of as-prepared sheet-like g-C3N4 supercell structure, is approximately 1.5 times higher than that of bulk g-C3N4.