Anodic Film Growth of Titanium Oxide Using the 3-Electrode Electrochemical Technique: Effects of Oxygen Evolution and Morphological Characterizations

Abstract

In the present study, potentiodynamic polarization scans followed by potentiostat anodizing tests have been employed to generate the anodic oxide films on commercially pure Ti in 1 M sulfuric acid and 1 M phosphoric acid. The highly stable single-barrier anodic films with a growth ratio of ∼1.5 nm V−1 (sulfuric acid) or ∼1.7 nm V−1 (phosphoric acid) were generated at the anodic voltages from 10 V to 60 V. During the potentiostatic anodizing, the anodic film was formed after the growth of the passive oxide film in the potentiodynamic polarization stage. Oxygen evolution proceeded within both the polarization and the anodizing stages, resulting in the suppression of the current efficiency for the growth of anodic films. The oxygen bubbles were induced by the amorphous-to-crystalline transition within the anodic film, leading to the formation of blister textures. Significant rupture of the anodic film was found that started at 20 V of the anodizing processes in the sulfuric acid; conversely, the significant rupture was started at 50 V in the phosphoric acid. The XRD results indicated that the degree of amorphous-to-crystalline transition in the anodic film formed in the phosphoric acid was less than the film formed in the sulfuric acid. The phosphate titanium oxide layers detected by XPS in the phosphoric acid indicated that more degrees of the amorphous-to-crystalline transition might be inhibited compared with the sulfated titanium oxides found in the sulfuric acid.