The first observation of titanate nanotubes by spherical aberration corrected high-resolution transmission electron microscopy

摘要

Multi-wall titanate nanotubes (MW-TNNTs) with high aspect ratio, large surface area and good uniformity were produced by alkaline hydrothermal treatment of grounded TiO_2 aerogels and further by applying freeze-drying. Not only the crystal phase and diameter, but also morphology of the starting materials impact on the aspect ratio and transformation efficiency of the obtained nanotubes. Other parameters, such as pH value during neutralization process and drying method for the final products, are important to control length and dispersion of MW-TNNTs. By spherical aberration corrected high-resolution transmission-electron-microscopy (Cs-corrected HRTEM) with lateral space resolution of 0.14 nm at 200 kV accelerating voltage and electron energy loss spectrum (EELS), the detailed structural analysis of MW-TNNTs reveals that (1) diameters of inner and outer tubes are about 4-7 nm and 10 nm, respectively, (2) numbers of layers are different from part to part along the longitudinal tube axis, (3) the walls of the tubes have interlayer spacing of 0.70-0.80 nm and the lateral fringes which are vertical to the walls have spacing of 0.32 nm, (4) eachrnlayer of MW-TNNT is the nanosheet composed by the arrayed TiO_6 octahedrons, and respective octahedron being slightly strained, and (5) no chirality of MW-TNNT tubular structure is observed.