Multilayer structure of tantalum anodic oxide films formed in dilute phosphoric acid

An investigation has been made of the multilayer structure of anodic oxide films on pure tantalum, formed up to various voltages with a constant current density of 1.0 mA cm^-2 in 1.0 × 10^-2 N H₃PO₄ at 20°C. For the study, infrared reflectance spectra (IRRS) were recorded and the optical thickness measuring method was successfully applied using the wavelengths of optical interference maxima and a chemical film stripper (concentrated ammonium hydrogen difluoride aqueous solution).The conclusions are that: (1) tantalum anodic oxide films anodized in dilute phosphoric acid consist of three layers, irrespective of the formation voltage; (2) the innermost layer is uniform whatever the anodization voltage; (3) phosphate anions are incorporated in both the outermost and middle layers but not in the innermost layer; (4) all three layers grow from the initial formation stage and the growth rates are nearly equal; (5) for formation voltages below 100 V the middle layer has an unchanging chemical structure, but above 100 V its chemical structure changes with the voltage; (6) the outermost layer appears to vary in chemical structure over all anodization voltages.