Adhesion measurement of highly-ordered TiO2 nanotubes on Ti-6Al-4V alloy

Self-assembled nanotubular arrays on Ti alloys could be used for more effective implantable devices in various medical approaches. In the present work, the adhesion of TiO2 nanotubes (TiO2 NTs) on Ti-6Al-4V (Ti64) was investigated by laser spallation and scratch test techniques. At first, electrochemical anodization was performed in an ammonium fluoride solution dissolved in a 90:10 ethane-1,2-diol (ethylene glycol) and water solvent mixture. This process was performed at room temperature (23°C) at a steady potential of 60 V for 1 h. Next, the TiO2 nanotubes layer was heat-treated to improve the adhesion of the coating. The formation of selforganized TiO2 nanotubes as well as the microstructural evolution, are strongly dependent on the processing parameters and subsequent annealing. From microscopic analysis, highly oriented arrays of TiO2 nanotubes were grown by thermal treatment for 90min at 500°C. Further heat treatment above 500°C led to the detachment of the nanotubes and the complete destruction of the nanotubes occurred at temperature above 700°C. Scratch test analysis over a constant scratch length (1000 μm) indicated that the failure point was shifted from 247.4 to 557.9 μm while the adhesion strength was increased from ~862 to ~1814mN after annealing at 500°C. The adhesion measurement determined by laser spallation technique provided an intrinsic adhesion strength of 51.4MPa for the TiO2 nanotubes on the Ti64 substrate.