Processing and Characterization of Functionally Graded Hydroxyapatite Coatings for Biomedical Implants

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Date

2010-08-07

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Abstract

Hydroxyapatite [Ca10(PO4)6(OH)2, HA] has been widely applied as a coating on various biomedical bone/dental implants to improve biocompatibility and bioactivity. It has been observed that primary reasons leading to implantation failure of commercial HA coated implants processed by plasma spraying are the poor mechanical properties of coatings and infections accompanied by implantation. It has been also reported an ideal coating should be able to stimulate new bone growth at the initial stage of implantation and stay stable both mechanically and chemically thereafter. This research has investigated a functionally graded hydroxyapatite (FGHA) coating that is capable of improving the stability of implants, facilitating recovery, and preventing infections after implantation. A series of FGHA coatings with incorporated Ag 0 ~ 13.53 wt. % has been deposited onto Ti substrate using ion beam assisted deposition (IBAD) with in-situ heat treatment. The compositional, microstructural, mechanical, and biological properties of coatings have been analyzed via various tests. The relationship among processing parameters, coating properties and biological behaviors has been established and the processing parameters for processing FGHA coatings with/without incorporated Ag have been optimized. Microstructure observations of coating cross section via transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) for set temperature coatings deposited at 450 oC ~ 750 oC reveals that in-situ substrate temperature is the primary factor controlling the crystallinity of the coatings. The microstructure observation of cross section via TEM / STEM for both FGHA coatings with / without incorporated Ag has shown that coatings are dense and have a gradually decreased crystallinity from substrate/coating interface to top surface. In particular, the interface has an atomically intermixed structure; the region near the interface has a columnar grain structure whereas the region near coating top surface is mostly amorphous. TEM / STEM observation of FGHA coating with incorporated Ag has also demonstrated that the metallic silver particles in size of 10 ~ 50 nm distribute at the coating cross section throughout the coating thickness. Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) analysis have shown that coatings consist of HA and various calcium phosphate compounds. The pull off tests have shown that the average adhesion strength of FGHA coatings (both with and without Ag) to substrate are in the range of 83.44 ± 5.71 ~ 89.36 ± 5.13 MPa. Further optical observation of pull off area of coating shows that no coating delamination is observed and epoxy failure is dominant, indicating a well-boned interface and a strong coating itself. It has been concluded that the high adhesion strength of coating to substrate is attributed to the atomic intermixed interface and dense structure of coating, which is resulted from the increased mobility of coating atoms at high substrate temperature under bombardment of assisted ion beam. Culture tests have shown a distinct increase in osteoblast cell attachment to FGHA surface after 24 hours culture test when compared to blank Ti controls. Both calcium and silver release tests of Ag-doped FGHA coatings have shown the release rate is high at the initial stage and it steadily decreases, which is the expected performance of FGHA coatings. Antibacterial test using S. aureus has revealed that Ag doped FGHA coatings show an inhibitory effect when compared to coating without Ag and blank Ti. In particular, with higher amounts of Ag in coatings, the inhibition of S. aureus is stronger. Cytotoxicity test indicates that the FGHA coating with the highest amounts of Ag shows a negative effect on the osteoblast response.

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Keywords

hydroxyapatite coating, biological properties, microstructural properties, mechanical properties, ion beam assisted deposition

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Degree

PhD

Discipline

Mechanical Engineering

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