SnO2 nanoparticles were found to self-pack at the air-hydrosol interface and form a nanoparticulate film. The self-packed films were observed under a Brewster angle microscope, and investigated by recording the time evolution of surface pressure and π-A isotherms. The results show that SnO2 nanoparticles take 3h to form a complete film at the air-hydrosol interface. Composite monolayers of SnO2 and arachidic acid were obtained by spreading arachidic acid onto a fresh hydrosol surface. Composite Y-type LB films were transferred from the air-hydrosol interface onto substrates, and characterized by FTIR, UV-vis, X-ray diffraction spectroscopy and TEM techniques. The results show that the composite films have good structure, with SnO2 nanoparticles uniformly and compactly distributed in the arachidate matrix.