Electrochemical deposition of calcium phosphate (CAP) on valve metals such as Ta, Nb, and Zr, was performed by anodic oxidation with alternate polarity inversion at an applied 20 VDC. A saturated hydroxyapatite(HAP)-phosphoric acid solution (pH 3) was used as the electrolyte. FTIR, XRD, and XPS were employed to investigate the detailed characteristics of the deposition. HAP was precipitated on Ta; HAP including brushite and monetite on Nb; and HAP and monetite on Zr. The Ca/P atomic ratios were 1.3-1.5 by XPS, and HPO4 2-bands were detected on Ta by FTIR. Therefore, the HAP precipitated on Ta was a Ca-deficient HAP. In addition, the XPS spectra of the specimens showed that phosphate ions were incorporated into the anodic oxide film. Deposits with nano-grain size were observed by AFM. The results confirmed that CAP with nano-grain size was deposited on valve metals by the anodic oxidation with polarity inversion.
To gain insight on the early biological response to commercial pure titanium (cpTi), the surface properties of cpTi implants retrieved from rat bone were examined by X-ray photoelectron spectroscopy (XPS). To this end, semi-cylindrical bullets, 1.1 mm in diameter and 3.5 mm in length, were implanted into the femurs of Wistar rats and then retrieved after either 3 hours or 7 days. Regardless of implantation interval, elements of Ti, O, C, and N were observed on the retrieved implants and that the thickness of the adsorbed film (mainly protein) was estimated to be about 2.5 nm. Small amounts of both Ca and P were also detected, whereby the Ca/P atomic ratios after 3 hours and 7 days were very small compared to that of hydroxyapatite. Furthermore, no correlation was found between the Ca and P distributions in the element maps. In conclusion, no calcium phosphate compounds were formed on the implant in vivo after 7 days.
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