The mechanism of phase separation of sol-gel alkoxy-derived silica sys
tems obtained by acid catalysis in the presence of poly(methyl methacr
ylate) (PMMA) and tetrahydrofuran was investigated by light scattering
. Spinodal decomposition (SD) was confirmed for systems with intermedi
ate PMMA/alkoxy compositions occurring with a simultaneous viscosity i
ncrease. The initial stages of phase separation followed the linear th
eory proposed by Cahn. For systems with low PMMA content, a behaviour
typical of nucleation and growth was detected. In this case gelation t
ook place after demixing. The morphology of the final PMMA/silica hybr
id material was investigated by scanning and transmission electron mic
roscopy with element-specific analysis. A matrix/disperse domains morp
hology was also verified for systems which demixed by SD, indicating t
hat phase coarsening occurs. A micellar/lamellar microstructure was ob
served inside the separated phases.