Organically modified MSU- x mesophases containing phenyl, ureidopropyl and methyl along with phenyl two moieties were directly prepared by one- pot synthesis method. Their texture and surface properties were characterized by means of XRD, HRTEM, FT- IR, N2 adsorption/desorption, 29Si CPMAS NMR、 13C CPMAS NMR and the microscopic structure was also characterized by small angle X- ray scattering (SAXS) using synchrotron radiation as X- ray source. The results showed that SAXS profiles were hardly constant with Porod′ s law showing a negative slope, i.e. negative deviations (see fig.3). This suggested that the organic groups covalently linked with the matrix of mesoporous silica formed an interfacial layers, which led to the scattering of the pore distortion and gave a negative diviation from Porod′ s law. The average thickness of the interfacial layer in each sample was further obtained by analyzing this deviation. SAXS analysis also showed that the organically functionalized MSU- X displayed mass fractal and the uniform distribution of the organic groups within the mesoporous channels, implying that it′ s formation was a non- equilibrium and non- linear process.