A versatile sol–gel synthesis route to metal–silicon mixed oxide nanocomposites that contain metal oxides as the major phase

The general synthesis of metal–silicon mixed-oxide nanocomposite materials, including a variety of both main group and transition metals, in which the metal oxide is the major component is described. In a typical synthesis, the metal-oxide precursor, MClx·yH2O(x=2–6,y=0–7), was mixed with the silica precursor, tetramethoxysilane (TMOS), in ethanol and gelled using an organic epoxide. The successful preparation of homogeneous, monolithic materials depended on the oxidation state of the metal as well as the epoxide chosen for gelation. The composition of the resulting materials was varied from M/Si=1–5 (mol/mol) by adjusting the amount of TMOS added to the initial metal-oxide precursor solution. Supercritical processing of the gels in CO2 resulted in monolithic, porous aerogel nanocomposite materials with surface areas ranging from 100–800m2g−1. The bulk materials are composed of metal oxide/silica particles that vary in size from 5–20nm depending on the epoxide used for gelation. Metal oxide and silica dispersion throughout the bulk material is extremely uniform on the nanoscale. The versatility and control of the synthesis method will be discussed as well as the properties of the resulting metal–silicon mixed oxide nanocomposite materials.