Published online by Cambridge University Press: 28 February 2011
Anhydrous sol-gel condensation of triethyl phosphate [(CH3CH2O)3PO] with boron trichioride (BCl3), triethyl aluminum [(CH3CH2)3Al] or silicon tetrachloride [SiCI4] in organic solvents led to rigid gels. The pore fluid of the gels was removed under supercritical conditions in a pressurized vessel to form porous solids. The condensation chemistry prior to the gel point was monitored by solution 1H, 13C, 31P, and 11B NMR. The materials were then calcined at progressively higher temperatures to produce high surface area phosphates. Nitrogen gasphysisorption was used to determine the surface areas, total pore volume, and average pore radius of the products. FT-IR was used to determine functional groups in the materials. The microstructure was also examined by scanning electron microscopy.