This thesis investigates the synthesis of ordered mesoporous silica and alumina materials with unique microstructures and different morphologies using novel approaches based on template-assisted synthesis and chemical vapor deposition (CVD) techniques and their potential use in polymer reaction application. Template-assisted growth of mesoporous silica under acidic and quiescent conditions at an oil-water interface can generate mesostructured silica with fibrous and non-fibrous morphologies. Fibers are obtained due to slow and one-dimensional diffusion of precursors through the interface. Variation in conditions can alter the axial growth of silica and yield non-fibrous shapes. Fibers grow from their base attached to the interface and coalesce to form fibers with larger diameters. Gas transport in silica fibers is governed by Knudsen and surface diffusion mechanisms. Surface diffusion contributes to 40% of the flow reflecting highly smooth pores. Real Knudsen and surface diffusivities are in the order of 10E-3 and 10E-5 cm2̂/s respectively. The one-dimensional mesopores are 45 time longer than the fiber length and align helically around the fiber axis with a pitch of 1.05 micron. Mesoporous silica membranes were prepared by a novel counter diffusion self assembly (CDSA) approach. This approach introduces the precursors from the opposite sides of a hydrophobic supports and yields silica plugs grown within its pores. Silica plugs grow with thickness of 0.5 mm and have a mesoporous structure. Such mechanically strong membrane is potential in protein separation and polymer reaction applications. Mesoporous membranes with controlled pore microstructure can be also obtained using cyclic CVD modification of straight 20 nm pore alumina membranes. Leaving residual of precursors in the pore after introduction of each precursor causes deposition of alumina in a fractal structure suitable for gas separation. Purging the pore after each precursor causes deposition in atomic layer with cylindrical mesopores suitable for membrane reaction applications. Titanocene-supported MCM-41 was used as molecular extruder for preparation of 60 nm polyethylene nascent fibers with extended-chain crystalline structures. The nascent fibers aggregate into 1-30 ư m microfibers which further aggregate into fiber bundles. Mechanical properties, measured for the first time, demonstrated an improved tensile strength of the polyethylene product compared to commercial polyethylene fibers.