Structural characteristics and residual stresses in oxide films produced on Ti by pulsed unipolar plasma electrolytic oxidation
Résumé
Oxide films, 7 to 10 μm thick, were produced on commercially pure titanium by plasma electrolytic oxidation in a sodium orthophosphate electrolyte using a pulsed unipolar current with frequency (ƒ) and duty cycle (δ) varied within f = 0.1 to 10 kHz and δ = 0.8 to 0.2 respectively. The coatings comprised a mixture of an amorphous phase with nanocrystalline anatase and rutile phases wherein the relative content of rutile varied from 17 to 25 wt%. Incorporation of phosphorus from the electrolyte into the coating in the form of PO2-, PO32- and PO43-, as demonstrated by EDX and FT-IR analyses, seems to contributed the formation of the amorphous phase. Residual stresses associated with the crystalline coating phase constituents were evaluated using the X-ray diffraction Sin2ψ method. It was found that, depending on the treatment parameters, internal direct and shear stresses in anatase ranged from -205 (±17) MPa to -431 (±27) MPa and from -98 (±6) MPa to -145 (±10) MPa respectively, whereas the rutile structure is comparatively stress free.
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