The interaction between azo dyes and cationic surfactant was studied by absorption spectroscopy and fluorescent Rayleigh scattering. In order to presume the structure of formed micelle, methyl orange and ethyl orange as azo dyes and cetyltrimethylammonium bromide (CTAB) as cationic surfactant were used. Infomations about interaction parameter including absorption maxima, optimal conditions, and intensity of fluorescent Rayleigh scattering were obtained. When azo dyes and CTAB are formed 1 : 1 complex, it showed the strongest intensity of fluorescent Rayleigh scattering. On going from mixed micelle to homomicell, It suggests successively several intermediate steps of complex structure which can be distinguished clearly from one another.