Interface feature characterization and Schottky interfacial layer confirmation of TiO2 nanotube array film

We report here characterization of the interfacial microstructure and properties of titanium dioxide (TiO2) nanotube array films fabricated by anodization. Field effect scanning electron microscopy (FESEM), Xray diffraction (XRD), nanoindentation, atomic force microscopy (AFM), selected area electron diffraction (SAED), and high-resolution transmission electron microscopy (HRTEM) were used to characterize the interface of the film. With increasing annealing temperature from 200 degrees C to 800 degrees C, the interfacial fusion between the film and the Ti substrate increased. The phase transformation of the TiO2 nanotube film from amorphous to anatase to rutile took place gradually; as the phase transformation progressed, the force needed to break the film increased. The growth of TiO2 nanotube arrays occurs in four stages: barrier layer formation, penetrating micropore formation, regular nanotube formation, and nanofiber formation. The TiO2 nanotubes grow from the Schottky interface layer rather than from the Ti substrate. The Schottky interface layer's thickness of 35-45 rim was identified as half the diameter of the corresponding nanotube, which shows good agreement to the Schottky interface layer growth model. The TiO2 nanotube film was amorphous and the Ti substrate was highly crystallized with many dislocation walls. (C) 2015 Elsevier B.V. All rights reserved.