Co-continuous morphology on spin coating produced thin TiO₂ films

Biological research has shown good cell response to dense TiO₂ films. Good surface chemistry of the implant can be further improved by introducing optimal topology, which in the case of osseointegration means porosity features in the nm and μm range. TiO₂ films are produced by spin coating and the obtained morphologies are characterized qualitatively and quantitatively from the scanning electron microscope images of the surface and in focused ion beam cross-sections. Infrared spectroscopy, thermogravimetry/differential thermal analysis, and X-ray diffraction were used to characterize chemical changes and crystallization processes in the bulk gels and thin films. Mechanical properties of the films are characterized using Nano Scratch Test. Results show that the increase in acetyl acetone (ACAC) concentration from 1 mol ACAC:1 mol Ti(IV) n-butoxide used for dense films to 1.5:1 and simultaneous polyethylene glycol (PEG) presence led to a change in morphology from a dense to highly porous, co-continuous morphology. This is a result of pronounced phase separation with respect to gelation due to (1) the presence of uncomplexed ACAC, which is highly dissimilar, in a sense of polarity, to the other components of the sol and (2) the additional reaction between PEG and TiO₂ oligomers. This porous morphology is found to be very sensitive to production parameters such as viscosity, spinning velocity and the amount of PEG added to the sol. It was also detected that, in addition to the phase separation, PEG also influences the crystallization process of the film.