A microemulsion was successfully prepared via polycondensation of alkoxy silanes. Research into the control of the preparation and properties of the microemulsion was conducted. The structure and properties of the microemulsion were characterized by transmission electron microscopy (TEM) and photon correlation spectroscopy (PCS). The variation in the temperature, the methods, and the amount of catalyst and surfactant was studied in relation to the properties of the final microemulsion.