Periodic Mesoporous Organosilicas (PMOs) have been used as precursors to produce porous Silicon Oxycarbide glasses after pyrolysis at 1000°C in inert atmosphere. Up to now only PMOs with cubic ordering could be successfully converted into an ordered mesoporous SiCO glass. In our work we prepared, under strong acidic media and using an inorganic salt, a PMO with cubic Fm3m phase starting from 1,2-bis(triethoxysilyl)ethane as organosilane and PluronicF127 as templating agent. The as-prepared PMO has been characterized by XRD (Synchrotron beamline), N 2 adsorption/desorption and multinuclear solid state NMR ( 29 Si, 13 C). After pyrolysis under argon flow the Fm3m phase is retained and the sample still displays a high surface area of 260 m 2 /g. Further characterizations were performed by 29 Si MAS NMR and at 1000°C the product can be described as a true SiCO glass with mixed SiC x O 4-x units (0x4).
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