Tuning anatase and rutile phase ratios and nanoscale surface features by anodization processing onto titanium substrate surfaces

Both the anatase (A) and rutile (R) phases of titanium oxide have shown enhanced antimicrobial and bioactivity levels but the specific A/R phase ratio needed for the best results is still unknown. In this study titanium samples were anodized to produce specific ratios of anatase and rutile phases within the oxide layers. Specific ratios produced included maximum A minimum R, minimum A maximum R, 50% A 50% R, minimum A minimum R, and a non-anodized titanium control group. Samples were characterized for phase distributions within the oxide layers, surface porosity, corrosion resistance, and bioactivity. Results indicated the targeted phase ratios were reproducibly achieved during the anodization process. Samples containing the highest levels of anatase showed the largest individual pore sizes, but a lower overall percent porosity value compared to samples containing higher rutile levels. EBSD examination of the anodized layer cross-sections provided valuable new spatial information on the distribution of anatase and rutile phases within the anodized layers. Highly porous oxide layers showed significantly higher corrosion rates compared to non-anodized titanium, but no significant differences were shown in the icorr values between samples containing primarily anatase phase, samples containing primarily rutile phase, and samples containing an approximate 50:50 mixture of the two phases. Minimum A minimum R samples showed substantially less porosity compared to the other anodization groups, a significantly lower oxide thickness, and comparable corrosion rates to non-anodized titanium. All samples within the study showed apatite production in simulated body fluid within the seven day test period indicating enhanced bioactivity.