The synthesis of mesostructured materials including mesoporous silica, carbon and carbon-silica nanocomposites has become one of the leading topics in materials science because the mesostructured materials carry many unique properties such as high surface area, large and controllable pore size and structures, uniform pore size distributions and large pore volumes, which make the mesoporous materials many potential applications, for example catalyst supports, adsorbent for large molecules, hydrogen adsorption media, etc Template synthesis, a unique approach that utilizes hard (preformed nanostructured inorganic frameworks or nanoparticles) and/or soft templates (liquid crystal phase of amphiphilic molecules) to organize precursor building blocks into large controllable structures, has emerged as the most promising method to fabricate mesostructured materials Besides the mesostructure control, functionalization of mesoporous materials has also been a focus, because the functionalized organic groups may provide mesoporous materials with improved surface properties This dissertation addresses the synthesis of mesoporous materials through template techniques including aerosol-assisted self-assembly and evaporation induced self-assembly methods. The functionalized mesoporous silica can be prepared by one-step co-condensation of TEOS and organosiline and co-assembly with amphiphilic molecular template. The mesostructure, pore size and morphology control can be realized by using different templates, synthesis methods and synthesis conditions. The content of hydrophobic molecule in the precursor solution also has dramatic effect on the mesostructures of obtained mesoporous silica particles. Both hard and soft templates are used to synthesize mesoporous carbon and carbon-based nanocomposites with tunable pore size, structures and morphologies. The applications of obtained mesoporous materials, such as catalysis and adsorption are discussed
