The experimental results on the synthesis and characterization of tetraethoxysilane (TEOS)/ methyltrimethoxysilane (MTMS)-based silica aerogels using two step sol-gel process via supercritical drying, are described. The obtained TEOS/MTMS-based aerogel showed properties of 0.1g/cm3 density, 95.5% porosity and 1070 m2/g specific surface area.