Ceramics-Silikáty 55 (4) 331-336 (2011)

SOL-GEL SILICA-BASED Ag–Ca–P COATINGS WITH AGRESSIVE PRETREATMENT OF TITANIUM SUBSTRATE

E. Borscheva, D. Horkavcová, Z. Cílová, A. Helebrant

The aim of the experiment was the obtaining of thin silica coatings on titanium by sol-gel method, using mechanical (SiC - paper No.180) and chemical (leaching in HF) pretreatments of the titanium substrates. The solutions were based on TEOS. For the sol-gel dipping process 4 different solutions were prepared: silica, silica with AgNO₃ and silica + AgNO₃ with brushite (CaHPO₄·2H₂O) or monetite (CaHPO₄) powders. The solutions were aged for 7 and 14 days at laboratory temperature. After sol-gel dip-coating process the samples were dried and fired. The adhesion of fired coatings was measured by tape test according to ASTM procedure and the bioactivity of the coatings was tested using in vitro test. The surfaces of the samples after firing, tape test and in vitro test were observed with the optical and electron microscopes. The firing results showed that silica-silver coatings did not change, brushite sol-gel coatings have cracked and the monetite sol-gel coatings have cracked also, but less than brushite ones. In spite of coating´s crackings, the square’s frames made on the surfaces were without any breakdowns after tape tests and the adhesion of all coatings was very good, classified by the highest grade 5. The results of in vitro tests showed that all coatings interacted with simulated body fluid (SBF). After exposition in SBF the new layer formed on substrates. In case of 7 days aged coatings containing brushite the new layer was uniform and compact. In case of 7 days aged coatings containing monetite the new layer was formed by crystals aggregated tightly together. The monetite and brushite coatings prepared from 14 days aged sol were the same as previous ones, but they were thicker. X-ray analyses after in vitro test confirmed dellaite, titanate and hydroxyapatite phases.

Keywords: Bioactive layers, Hydroxyapatite, Sol-gel method, Titanium, SBF, Tape-test