Influence of annealing temperature on RF magnetron sputtered calcium phosphate coatings.

The effect of different annealing temperatures on the characteristics of thin calcium phosphate coatings fabricated by radiofrequency magnetron sputtering was studied. Annealing of the as-sputtered films was necessary to change the amorphous coating to a crystalline coating. The films were annealed for 2 and 4 h at 400, 600, 800, 1000 and 1200 degrees C under dry argon or argon and water vapour flow. After annealing, the structure and the chemical composition of these films were characterized with incident light microscopy, Rutherford backscattering spectrometry (RBS), X-ray diffraction (XRD), and Fourier transform infrared absorption spectrometry (FTIR). Incident light microscopy showed cracks in the coatings annealed at a higher temperature than 400 degrees C. RBS revealed that the as-sputtered coatings had a high Ca/P ratio which decreased with increasing annealing temperature. After annealing at a temperature of 600 degrees C or more the XRD showed crystalline hydroxyapatite (HA) coatings. However, the second phase, present in the coatings, changed from tetra-calcium phosphate to calcium oxide to beta-tri-calcium phosphate with increasing annealing temperature. FTIR measurements showed the existence of OH- and PO- bonds in all coatings, although the PO- bonds varied for different annealed coatings, from the PO- bonds due to HA to PO- bonds due to other calcium phosphates. From the results of this study we suggest that 600 degrees C is probably the best annealing temperature to obtain a better characterization and understanding of the coating.

In vivo dissolution behavior of various RF magnetron-sputtered Ca-P coatings on roughened titanium implants.

RF magnetron sputter deposition was used to produce 0.1, 1.0 and 4.0 microm thick Ca-P coatings on TiO(2)-blasted titanium discs. Half of the as-sputtered coated specimens were subjected to an additional infrared heat treatment for 30s at 425-475 degrees C. X-ray diffraction demonstrated that infrared radiation changed the amorphous 4 microm sputtered coatings into an amorphous-crystalline structure, while the amorphous 0.1 and 1 microm changed in a crystalline apatite structure with the presents of tetracalciumphosphate as a second phase. Scanning electron microscopically examination of the sputtered coatings revealed that annealing of the 4 microm thick coatings resulted in the appearance of small cracks. Subsequently, the discs were implanted subcutaneous into the back of rabbits. After 1, 4, 8 and 12 weeks of implantation, the implants were retrieved and prepared for histological and physicochemical evaluation. Histological evaluation revealed that the tissue response to all coated implants was very uniform. A very thin connective tissue capsule surrounded all implants. The capsule was usually free of inflammatory cells. At the interface, there was a close contact between the capsule and implant surface and no inflammatory cells were seen. Physicochemical evaluation showed that the 0.1 and 1 microm thick amorphous coatings had disappeared within 1 week of implantation. On the other hand, the 4 microm thick amorphous phase disappeared during the implantation periods, which was followed by the precipitation of a crystalline carbonate apatite. Further, at all implantation periods the heat-treated 1 and 4 microm thick coatings could be detected. Occasionally, a granular precipitate was deposited on the heat-treated 4 microm thick coating. Fourier transform infrared spectroscopy showed the formation of carbonate apatite (CO(3)-AP) on the 4 microm thick amorphous coating and on the heat-treated specimens. On basis of our findings, we conclude that 1 microm thick heat-treated Ca-P sputter coating on roughened titanium implants appear to be of sufficient thickness to show bioactive properties, under in vivo conditions.

[Preserving alveolar bone with submucosal hydroxyapatite]. / Submucosale korrelvormige hydroxylapatietimplantaten.

In this article the use of hydroxyapatite granules to prevent alveolar bone loss after extraction of teeth is described. Twenty-six alveoli were treated in the mandible and the maxilla. The used method resulted in a delayed healing of the wound and loss of a part of the implants. On the account of the results it is recommended to close the extraction wound completely when using hydroxyapatite granules and to limit the indication to the mandible.

Study of the surface characteristics of magnetron-sputter calcium phosphate coatings.

Plasma-sprayed hydroxylapatite coatings on metals such as titanium have been investigated for many years and have shown a good biocompatibility when implanted in bony tissues. Radiofrequency magnetron sputtering was used as an alternative method to deposit thin films of hydroxylapatite on titanium substrates. X-ray diffraction demonstrated that the sputtered layer was crystalline with a preferred (001) crystallographic orientation with the C-axis perpendicular to the substrate surface. Scanning electron microscopy showed that the deposited films had a uniform and dense structure. The calcium phosphate ratio varied between 1.5 and 2.0, as determined by energy-dispersive X-ray analysis. The in vitro dissolution appeared to be determined by the degree of the coating's crystallinity.

Influence of discharge power level on the properties of hydroxyapatite films deposited on Ti6A14V with RF magnetron sputtering.

The effects of discharge radiofrequency (RF) power and film thickness were studied on the characteristics of Ca5(PO4)3OH (hydroxyapatite) thin films fabricated by RF magnetron sputtering. The structure and chemical composition were investigated with alpha-step (thickness), scanning electron microscopy (SEM), X-ray diffraction (XRD), Rutherford backscattering spectrometry (RBS), and infrared absorption spectrometry (FTIR). The films were analyzed as-sputtered and after annealing at 550 degrees C under argon flow. SEM showed that the film surfaces had no cracks or other defects. X-ray diffraction showed that the deposited films were amorphous with low-discharge RF power, and crystalline with high-discharge RF power. After annealing, all the films had the same crystalline structure as apatite. However, the RBS measurements revealed that all films had a higher calcium-phosphate ratio than standard synthetic hydroxyapatite. Furthermore, statistical testing of the RBS data revealed the existence of only a weak correlation between the Ca/P ratio and the discharge power level. Although all sputtered films showed phosphate bonds in the infrared spectrum, only after annealing did the OH bonds of hydroxyapatite become visible.