Thin films of bicontinuous cubic mesostructured silica were formed using the nonionic poly(oxyethylene)- alkyl ether surfactant Brij-56 as a structure-directing agent. The synthesis conditions were chosen such that the estimated volume fraction of surfactant in the silica/surfactant films corresponded approximately to the composition at which the bicontinuous cubic phase occurs in the water/surfactant phase diagram. Small-angle X-ray scattering and transmission electron microscopy measurements reveal that the cubic phase corresponds to the Iad double-gyroid structure, with some distortion due to anisotropic film shrinkage. The cubic structure grows as faceted domains that are well-oriented with respect to the substrate and often occur in coexistence with a lamellar phase. By adjusting the temperature at which the films are aged, it is possible to create films with 2D hexagonal, cubic, or lamellar structures at a single composition. microscopy and X-ray diffraction showed that well ordered internal 2D hexagonal mesostructures could be prepared using both nonionic block copolymers and cationic surfactants as the templating molecules. Disordered cubic and well ordered lamellar, onion like, particles were prepared from the block copolymer templates. Nitrogen sorption data and mercury porosimetry show that pore size distribution of the mesoporous particles is very narrow with pore sizes varying from 2.5 to 8.5 nm as a function of templating amphiphiles. We have shown that the mesoscopic pores are accessible after calcination and can be filled with relatively large molecules; the particles adsorbed more than 20% (by weight) of the cationic dye Janus Green B from aqueous solutions.