Abstract-Biocompatible silica aerogel microparticles are promising drug delivery vehicles because of their large surface area and open pore structures. A simple process has been developed in this work to prepare silica aerogel microparticles from rice husk ash, using water-in-mineral oil emulsion for sol-gel, followed by aging in ethanol to strengthen gel network and drying with scCO 2 . This process obviates drawback of current methods for silica aerogels. The effects of speed of agitation of water-oil mixture, sol-to-oil ratio and surfactant concentration have been investigated on particle size and size distribution, BET surface area, cumulative pore volume and pore diameter. A surface area of 654 m 2 /g, higher than the values reported for similar materials, could be obtained.Index Terms-Rice husk ash, silica aerogel microparticles, supercritical carbon dioxide, water-in-oil emulsion.