Complementary techniques, including nitrogen adsorption, small-angle X-ray scattering (SAXS), and atomic force microscopy (AFM), have been utilized to characterize the surface features of highly microporous carbon materials prepared from highly aromatic polymers. Nitrogen adsorption measurement interpreted by BET, DR, HK, and NLDFT methods reveals these nanostructured activated carbons exhibit a high surface area of up to 4000 m2/g, a micropore volume up to approximately 1.75 mL/g, and an average pore size of approximately 10-20 angstroms. A modified equation, based on Porod's law, the Debye-Bueche equation, and fractal dimension theories, has been proposed and successfully applied to analyze the SAXS spectra and to extract the porous texture of these unique activated carbons. AFM 3D imaging combined with the Fourier transform technique has been applied to statistically quantify pore sizes on the carbon surface.