Multistep structural transition of hydrogen trititanate nanotubes into TiO2-B nanotubes:: a comparison study between nanostructured and bulk materials

H-trititanate nanotubes obtained by alkali hydrothermal treatment Of TiO2 followed by proton exchange were compared to their bulk H2Ti3O7 counterpart with respect to their thermally induced structural transformation paths. As-synthesized and heat-treated samples were characterized by XRD, TEM/SAED, DSC and spectroscopy techniques, indicating that H2Ti3O7 nanotubes showed the same sequence of structural transformations as their bulk counterpart obtained by conventional solid state reaction. Nanostructured H2Ti3O7 converts into TiO2(B) via multistep transformation without losing its nanotubular morphology. The transformation occurs between 120 and 400 degrees C through topotactic mechanisms with the intermediate formation of nanostructured H2Ti6O13 and H2Ti12O25, which are more condensed layered titanates eventually rearranging to TiO2(B). Our results suggest that the intermediate tunnel structure H2Ti12O25 is the final layered intermediate phase, on which TiO2(B) nucleates and grows. The conversion of nanostructured TiO2(B) into anatase is completed at a much lower temperature than its bulk counterpart and is accompanied by loss of the nanotubular morphology.