Self-assembled nonionic alkyl glycoside surfactants are of interest for creating functional adsorption and catalytic sites at the surface of mesoporous sol-gel-derived materials, but they typically impart poor long-range order when they are used as pore templates. Improved order and control over the functional site density can be achieved by mixing the alkyl polyglycoside surfactant with a cationic surfactant. Here, we investigate the rarely reported lyotropic liquid crystalline (LLC) phase behavior of aqueous solutions of a nonionic disaccharide surfactant, n-dodecyl-beta-D-maltoside (C(12)G(2)/DM), and cetyltrimethylammonium bromide (C(16)TAB) by low-angle powder X-ray diffraction (XRD) and polarized optical microscopy (POM). An approximate ternary phase diagram of the C(16)TAB-C(12)G(2)-water system is developed at 50 degrees C, which includes 2-D hexagonal (P6mm symmetry), bicontinuous cubic (Ia (3) over bard symmetry), lamellar, and rectangular (cmm symmetry) LLC phases. By replacing the volume of water in the phase diagram with an equivalent Volume of silica, ordered mesoporous materials are prepared by a nanocasting technique with variable C(12)G(2)/C(16)TAB ratios. For large regions of the phase diagram, this approach is predictive. However, silica materials synthesized with comparatively high C(12)G(2)/C(16)TAB ratios are only poorly ordered in a way that does not correspond to their lyotropic liquid crystalline phase behavior. Also, in contrast with our previous Study of mixed C(16)TAB/n-octyl-b-D-glucopyranoside templating [37] the boundary between hexagonal and bicontinuous cubic materials is shifted towards higher surfactant content than in the aqueous LLC system. (C) 2009 Elsevier Inc. All rights reserved.