Microheterogeneity in phenyl group modified inorganic/organic hybrid gels after aerosol drying or slow solvent evaporation

► Slow drying sol-gel processing produces heterogeneous amorphous materials, and fast spraydrying generates homogeneous gels. ► Cross polarization dynamics distinguishes between homogeneous and heterogeneous silica gels. ► Phenyl functionalized hybrid gels form porous silica after calcinations.