Effect of fluoride and water content on the growth of TiO2 nanotubes synthesized via ethylene glycol with voltage changes during anodizing process

In this work, titanium foils were anodized in ethylene glycol solutions containing different amounts of water and fluoride to determine their effects on the top morphology and crystalline structure of the formed titania nanostructures. Anodizing was performed for 2 h by using titanium foils as both anode and cathode applying a squared-pulse voltage profile composed of one step at 80 V for 3 min followed by another at 20 V for 5 min; constant voltage conditions were also used to study the nanostructure formation on the surface. We found the formation of nanostructured titania on the surface of the anodized foil when small amounts of water and fluoride are present in the anodizing solution. The top of these nanostructures is irregular when no water is added, but is expected to change with different amounts of water and fluoride in the ranges of 1 - 9% and 0.05 - 0.5%, respectively. Synthesis parameters also change nanotube morphology. The morphology and structure properties of the samples were studied by scanning electron microscopy (SEM) and X-ray powder diffraction (XRD). Formation of TiO₂ nanotubes by anodization method are strongly correlated to conditions like fluoride concentration and applied voltages. Tube length varying between 2 and 7 μm, exhibiting different diameters and wall thicknesses were obtained. When an alternate voltage was applied, the wall of the nanotubes presented evenly spaced rings while nanotubes with smooth wall form were observed when constant voltage was applied. Reflection peaks corresponding to Brookite, Anatase, and Rutile of TiO₂ phases were observed from XRD measurements. A correlation between the effects of synthesis parameters on nanotube formation and morphological properties is presented. TiO₂ nanotubes prepared by electrochemical anodization have excellent performance in various applications such as photocatalysts, solar cells, gas sensors, and biomedical applications.