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The TiO2/vermiculite composites were prepared by in-situ hydrolyzing reaction and in-situ dehydrating reaction of tetrabutyl titanate-hexadecyl trimethyl ammonium bromide intercalated vermiculite.The structural phase transition of TiO2 in TiO2/vermiculite composites calcined at different temperatures was characterized by using XRD and Raman.The results show that at calcination temperature of 800℃ appeared the anatase phase of TiO2 in TiO2/vermiculite nanocomposites, while pure TiO2 is all converted to rutile at the same temperature.