Anionic surfactant sodium lauryl sulfate（SDS）, cationic surfactant palmityl trimethyl ammonium chloride（CTAC） and TiO2 were used to prepare multilayer films on quartz optic fibers by the electrostatic self-assembly （ESA） method. The whole self-assemble process, the function of surfactant and the effect of TiO2 slurry′s concentration to the self-assemble were discussed. The isoelectric point of TiO2 slurry measured by experiment is 6.8. The results show that whatever the concentration of the TiO2 dispersion, a flat and compact adsorbed monolayer on the optic fiber can be built in a stable dispersion at lower pH. There is a adsorbed equilibrium on the substrate （fiber）/solution interface when enough time of incubation is given. A rough and loosen adsorbed layer is formed on the fiber surface by immersed the substrate in a high pH dispersion （pH>10） because the presence of hydroxyl on particle surface. Film thickness can be controlled by controlling the number of layers in the film.
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