Phase behavior for the mixed aqueous surfactant systems of cationic octadecyl trimethyl ammonium chloride (OTAC)/anionic ammonium dodecyl sulfate (ADS)/water was examined. Below the total surfactant concentrations of 1.5 m molal, mixed micelles were formed. At the total surfactant concentrations higher than 1.5 m molal, there appeared a region where mixed micelles and vesicles coexist. As the surfactant concentration increased, the systems looked very turbid and much more vesicles were observed. The vesicles were spontaneously formed in this system and their existence was observed by negative-staining transmission electron microscopy (TEM), small-angle neutron scattering (SANS) and encapsulation efficiency of dye. The vesicle region was where the molar fraction α of ADS to the total mixed surfactant was from 0.1 to 0.7 and the total surfactant concentration was above 5 × 10-4 molality. The size and structure of the vesicles were determined from the TEM microphotographs and the SANS data. Their diameter ranged from 450 nm to 120μm and decreased with increasing total surfactant concentration. The lamellar thickness also decreased from 15 nm to 5 nm with increasing surfactant concentration and this may be responsible for the decrease in vesicle size with the surfactant concentration. The stability of vesicles was examined by UV spectroscopy and zeta potentiometry. The vesicles displayed long-term stability, as UV absorbance spectra remained unchanged over two months. The zeta potentials of the vesicles were large in magnitude (40-70 mV) and the observed longterm stability of the vesicles may be attributed to such high ζ potentials.