Influence of thermal treatments in nanotubular anodic coatings of TiO2
ABSTRACT TiO2 is a semiconductor widely used in heterogeneous photocatalysis processes for water decontamination. Several studies indicate that ordered nanostructures in anatase phase improve the photocatalytic properties with respect to other morphologies and crystal structures of TiO2. The aim of the present work is to evaluate the influence of different thermal treatments on the structural integrity and crystal structure of the nanotubular TiO2 coatings synthesized by the anodic oxidation technique. A solution of 0.6% w/w ammonium fluoride and 3.5% w/w water in ethylene glycol was used as the electrolyte for the oxidation. A direct current was used at a constant voltage of 45 V during 2 h. After the anodic oxidation, thermal treatments of 2 h and 4 h at 450, 550 and 650 °C with a heating ramp of 10 ºC/min were performed. Morphology and crystalline structure of the coatings were characterized by scanning electron microscopy and X-ray diffraction, respectively. TiO2 coatings of nanotubes about 85 nm inner diameter, 18 nm wall thick and 7 ?m in length (mean value) were obtained. The nanotubes maintained their structural integrity without changes in the dimensions with the applied thermal treatments. However, the morphology of the walls of the nanotubes was modified with the time and temperature of the thermal treatments, evidencing the formation of anatase crystals. Even on the coatings thermally treated at 550 °C, nanocrystalline anatase deposits on the outside wall of the nanotubes were observed. Regarding the crystal structure, the coatings were amorphous previously to the thermal treatments and were crystalline in anatase phase after thereof, indicating the anatase stabilization even up to 650 °C, temperature at which the rutile phase appeared.