S. Lederer, P. Lutz, W. Fürbeth
Surface & Coatings Technology 335 (2018) 62-71
Titania coatings were produced on Ti 13Zr 13Nb by a unipolar pulsed DC plasma electrolytic oxidation (PEO) process in an electrolyte containing 1 M H2SO4 + 0.1 M H3PO4. The samples were galvanostatically anodized under a constant charge-carrier density of 63 C cm− 2 and current-densities reaching from 14 mA cm− 2 up to 700 mA cm− 2. Both a constant current mode and a unipolar pulsed mode with a duty-cycle of 50% and frequencies of 1 Hz to 50 Hz were performed. The surface layers were characterized by scanning electron microscopy (SEM/EDX), X-ray diffraction (XRD) and nanoindentation. Titanium oxide coatings with a thickness of several micrometers and a porous structure could be generated. The coatings morphology was evaluated. It can be shown that the porosity can be reduced with increasing frequency. The coatings consist of anatase and rutile, the phase composition of the coatings can be adjusted by the PEO current density. The corrosion resistance of the layers was tested in a simulated body fluid (SBF) with the addition of 0.1 M H2O2 by open circuit potential measurements, potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). EIS data fitting indicates a composed layer structure of an outer porous layer and an inner barrier layer. Higher current densities during the PEO process formed thicker coatings, which consequently resulted in lower corrosion currents. The addition of zirconia nanoparticles into the electrolyte increased the surface hardness to an average value of 12.8 GPa, compared to that of an untreated sample (4.1 GPa) and PEO samples without particle addition (8.5 GPa).