Abstract SnO 2-pillared titanate nanohybrid has been prepared by reacting the exfoliated layered titanate sheets with the nanosized SnO 2 sol particles. The stable two-dimensional colloidal nanosheets could be obtained by intercalating tetrabutylammonium cation into the layered protonic titanate, H x Ti 2− x/4 □ x/4 O 4·H 2O ( x=0.67) with a lepidocrocite-like structure, and by successive exfoliation process in an aqueous solution. Monodispersed SnO 2 nano sol particles were prepared by hydrolysis of SnCl 4·5H 2O in the presence of sodium hydroxide, and then the exfoliated titanate suspension was mixed with SnO 2 nano sol solution until the flocculated products formed. The final product was heated at various temperatures in order to complete the grafting reaction of intercalated SnO 2 nano sol on the interlayer surface of layered titanate. Inductive coupled plasma, X-ray diffraction, thermal analysis and N 2-adsorption–desorption isotherms were carried out to study the hybridizing process and the structure of SnO 2-pillared titanate nanohybrid.