GELATION OF N3P3[NH(CH2)3Si(OEt)3]6-n [X]n X = NH(CH2)3Si(OEt)3, NCH3(CH2)3CN AND OC6H4(CH2)CN, n = 0 or 3 at the LIQUID/AIR/INTERFACE

Abstract

The compounds N3P3[NH(CH2)3Si(OEt)3]6 (1), N3P3[NH(CH2)3Si(OEt)3]3[NCH3(CH2)3CN]3 (2) and N3P3[NH(CH2)3Si(OEt)3]3 [HOC6H4(CH2)CN]3 (3) undergo slow gelation at the interface oil/air at low temperatures to give perfect gels G1, G2 and G3 respectively. TEM analysis reveals nanoparticles of silica with mean size of about 10 nm. Pyrolysis under air at 800 °C of these gels affords a mixture of mainly Si5(PO4)6O, SiP2O7 and SiO2. Gelation and pyrolysis products were characterized by IR, solid-state NMR, TEM, SEM-EDAX microscopy and X-ray diffraction. The sol-gel process in the interface liquid /air is discussed in comparison with the usual sol-gel solution process.