Abstract. The thin calcium-phosphate (Ca-P) coatings produced by the ion-beam-mixing method instead of the plasma-spraying method have been found to be amorphous, resulting in films that easily dissolved in simulated body fluid. These coatings crystalized with conventional heat treatment in an electric furnace but tended to crack easily. Therefore, the purpose of this study was to find a suitable heat treatment that controls the solubility of Ca-P coatings without weakening their adhesion to titanium (Ti) substrate.Thin coatings (approximately 1 lim) were coated onto Ti substrates, followed by heat treatment in a conventional furnace and rapid heating by infrared radiation and laser radiation. X-ray diffraction analysis revealed untreated films to be amorphous but to become crystalline after being heated in a fumace at 500'C, heated rapidly with infrared radiation higher than 600°C and with laser radiation at output power of 10W. We evaluated solubility by estimating the film thickness after immersion in simulated body fluid for 5 weeks: Untreated films dissolved within 1 day. Coatings treated with infrared radiation at 600°C dissolved minimally. Cracks were observed in coatings subjected to infrared radiation at 800°C and fumace-heated at 500°C. Coatings treated with laser radiation tended to dissolve easily, with non-uniform surface degradation. Xray photoelectron spectroscopy analysis at the interface between the coating and the Ti substrate showed that cracks were the result of decreased Ca-implanted layers and too much growth of Ti-P compounds. No difference was recognized in the Ti-oxidation state among specimens. These data indicate that rapid, homogeneous, and comparatively low-temperature heating, such as defocused infrared radiation, controls Ca-P solubility and ensures the adherence of the coatings to the substrate.
The morphological relationship between titanium and lysosomal proteinases, cathepsins B and D, at the bone-titanium interface using titanium-coated plastic implants placed for 28 days in the tibiae of 6-week-old rats was immunocytochemically investigated by the colloidal immunogold-silver method. Under light microscopy the titanium layer appeared to make direct contact with the bone and one or a few layers of slender cells were interposed between the bone and titanium. Ultrastructurally, the titanium came in contact with the bone or the slender cell layer through a 20 to 40 nm thin amorphous zone. The slender cells at the bone-titanium interface consisted of two types; one was an osteoblast type with glycogen granules which was found along the newly-formed bone facing titanium layer. The other was a fibroblast type which came in contact with the titanium layer and occasionally endocytosed the detached titanium fragments. In addition, some of the slender cells also showed degenerative changes. Immunocytochemically, cathepsins B and/or D were sometimes colocalized in some phagolysosomes with titanium fragments. These findings suggested that the fibroblast types at the bone-titanium interface may act as scavengers to remove both cell debris and titanium by means of some endocytotic ability, and lysosomal cathepsins also developed in response to the endocytosed titanium. The osteoblast type also appears to show a high degree of osteogenic activity around the titanium-coated plastic implants.
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