BaTiO3 (BTO) layers were deposited by pulsed laser deposition (PLD) on TiNb, Pt/TiNb, Si (100), and fused silica substrates using various deposition conditions. Polycrystalline BTO with sizes of crystallites in the range from 90nm to 160nm was obtained at elevated substrate temperatures of (600°C-700°C). With increasing deposition temperature above 700°C the formation of unwanted rutile phase prevented the growth of perovskite ferroelectric BTO. Concurrently, with decreasing substrate temperature below 500°C, amorphous films were formed. Post-deposition annealing of the amorphous deposits allowed obtaining perovskite BTO. Using a very thin Pt interlayer between the BTO films and TiNb substrate enabled high-temperature growth of preferentially oriented BTO. Raman spectroscopy and electrical characterization indicated polar ferroelectric behaviour of the BTO films.
Ti-doped hydrogen free diamond-like carbon (DLC) layers of dopation up to ~25 at.% were prepared by dual beam pulsed laser deposition (PLD) using two excimer lasers. The arrangement allows continuous fine tuning of dopant concentration on a large scale and deposition flexibility. The layers were prepared on Si(1 0 0) and Ti6Al4V substrates at room temperature. The surface morphology, mechanical properties, bonds, composition, morphology of human osteoblast-like Saos-2 cells, their metabolic activity and production of osteocalcin, a marker of osteogenic cells' differentiation were tested. The films' composition changed after x-ray photoelectron spectroscopy (XPS) surface cleaning by argon clusters. Adhesion moved with Ti dopation from 4 N (DLC film) to 11 N (25 at.% of Ti in DLC). Creation of TiC was observed for higher Ti dopation. The contact angle and surface free energy stayed unchanged for higher Ti dopation. Saos-2 cells had the highest metabolic activity/viability on DLC with 10 at.% of Ti and on control polystyrene dishes on days 1 and 3. The Ti dopation improved the formation of vinculin-containing focal adhesion plaques in Saos-2 cells. Immunofluorescence staining revealed similar production of osteocalcin in cells on all tested samples.
Beta-titanium alloys are promising materials for bone implants due to their advantageous mechanical properties. For enhancing the interaction of bone cells with this perspective material, we developed a ferroelectric barium titanate (BaTiO3) coating on a Ti39Nb alloy by hydrothermal synthesis. This coating was analyzed by scanning electron and Raman microscopy, X-ray diffraction, piezoresponse force microscopy, X-ray photoelectron spectroscopy, nanoindentation, and roughness measurement. Leaching experiments in a saline solution revealed that Ba is released from the coating. A progressive decrease of Ba concentration in the material was also found after 1, 3, and 7 days of cultivation of human osteoblast-like Saos-2 cells. On day 1, the Saos-2 cells adhered on the BaTiO3 film in higher initial numbers than on the bare alloy, but they were less spread, and their initial proliferation rate was slower. These cells also contained a lower amount of beta1-integrins and vinculin, i.e., molecules involved in cell adhesion, and produced a lower amount of collagen I. This cell behavior was attributed to a higher surface roughness of BaTiO3 film rather than to its potential cytotoxicity, because the cell viability on this film was very high, reaching almost 99%. The amount of alkaline phosphatase, an enzyme involved in bone matrix mineralization, was similar in cells on the BaTiO3-coated and uncoated alloy, and on day 7, the cells on BaTiO3 film attained a higher final cell population density. These results indicate that after some improvements, particularly in its roughness and stability, the hydrothermal ferroelectric BaTiO3 film could be promising coating for improved osseointegration of bone implants.