The concentration vs composition diagram of aggregate formation of the dodecyltrimethylammonium bromide(DTAB) and didodecyldimethylammonium bromide (DDAB) mixture in aqueous solution at rather diluteregion was constructed by analyzing the surface tension, turbidity, and electrical conductivity data and inspectedby cryo-TEM images and dynamic light scattering data. Although the aqueous solution of DTAB forms onlymicelles, the transition from monomer to small aggregates and then to vesicle was found at 0.1 <
X2 1,where
X2 is the mole fraction of DDAB in the DTAB-DDAB mixture, while vesicle particles were formeddirectly from monomer solution at 0 <
X2 < 0.1. Furthermore, the transition from vesicle to micelle wasfound at 0 <
X2 < 0.4 at higher concentrations. An addition of DTAB to DDAB solution lowered considerablythe DDAB concentration of the vesicle formation, which is attributable to asymmetric distribution of DTABmolecules between inner and outer monolayers of the vesicle bilayer. The shape and size of aggregates wereobtained from surface tension, cryo-TEM, and light scattering data.