The hydrolysis and initial polycondensation processes of methyltriethoxysilane (MTES) have been investigated by high-resolution 29Si-nuclear magnetic resonance spectroscopy (29Si-NMR). MTES was hydrolyzed in the system with MTES:ethyl alcohol:water:HCL = 1:4:x:y; x = 1, 2, 3, 6; y = 1 × 10-4, 1 × 10-2. Signals due to end and middle groups of polysiloxanes formed sub-regions on the basis of the number of hydroxyl groups attached to silicon, and the sub-region for silicon possessing more hydroxyl groups was observed at a lower field. Based on signal intensities, the signals due to the dimers (Me(HO)2SiOSi(OH)2Me and Me(HO)2SiOSi(OH)OEt)Me) and the trimer (Me(HO)2SiOSiMe(HO)OSi(OH)2Me) (MeCH3, EtC2H5) were identified.
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