Chih-hao Yang

Plasma spraying of zirconia-reinforced hydroxyapatite composite coatings on titanium: part I: phase, microstructure and bonding strength.

Plasma-sprayed hydroxyapatite (HA) coatings applied to metal substrates can induce a direct chemical bond with bone and hence achieve biological fixation of the implant. However, the poor bonding strength between HA and substrate has been of concern to orthopaedists. In this study, two submicrometre ZrO2 powders stabilized with both 3 and 8 mol% Y2O3 (TZ3Y and TZ8Y, respectively) were incorporated in a plasma-sprayed HA coating on Ti-6Al-4V substrate to investigate the change in phase, microstructure and bonding strength. The results show that ZrO2 composite coatings contain more unmelted particles and greater porosity. During plasma spraying, ZrO2 reacts with the CaO in HA to form CaZrO3 and accelerates HA decomposition to α-TCP and Ca4P2O9. Nevertheless, bonding strength increases with increase of ZrO2 content in the range 0 to 10 wt% studied. The higher Y2O3-containing TZ8Y apparently exerts a greater strengthening effect than the lower Y2O3-containing TZ3Y.

Intramedullary implant of plasma‐sprayed hydroxyapatite coating: An interface study

An intramedullary implant model in the canine femora was developed to evaluate the mechanical and histological responses between cancellous bone and plasma-sprayed hydroxyapatite coatings (HACs) on ti-6A1-4V implants, with 12- and 24-week follow-ups. HACs of different thicknesses were investigated. Results of the mechanical testings revealed that after 24 weeks of implantation, the mean shear strength (2.49 +/- 0.12 MPa) of the 50 microns HACs was significantly higher (p < 0.05) than that of the 200 microns HACs (1.44 +/- 0.19 MPa). However, using backscattered electron images (BEIs) throughout all the implant periods, no substantial histological variations in the extent of new bone apposition between the two HACs were observed. Occasionally, solution-mediated disintegration of the 50 microns HAC was found 24 weeks postimplantation. Histomorphometric studies from the BEIs demonstrated that for both HACs the percentage of the direct HAC-cancellous bone contact was approximately 50% at 12 weeks and 75% at 24 weeks. After the mechanical tests, the 200 microns HACs had fracture sites either inside the coating layers or at the HAC-titanium interfaces, which might explain why the mechanical performance of the 200 microns HACs was inferior to that of the 50 microns HACs even though both HACs had the same histological behaviors.

SURFACE CHARACTERISTICS OF TI6AL4V ALLOY : EFFECT OF MATERIALS, PASSIVATION AND AUTOCLAVING

The properties of passivated films for Ti6Al4V alloy prepared by various methods (as-polished, brazed at 970 °C for 2 h and brazed at 970 °C for 8 h) were investigated. Four passivations (non-treated, nitric acid passivation, 400 °C-treated in air, and aged in boiling water), with or without autoclaving treatments, were adopted for evaluating the changes of surface properties, including chemical composition, chemical structure, and oxide thickness. From X-ray photoelectron spectroscopic (XPS) analyses, surface elements of copper and nickel in brazed samples were undetected for non-treated, acid-passivated and boiling water-aged specimens, while they were found in the 400 °C-treated specimen. The relative contents of Ti2++Ti3+ to Ti4+ were determined by passivation treatments, but were not related to the experimental materials and autoclaving treatment. Passivation and autoclaving decreased the Ti to Ti4+ ratio by virtue of an increase in oxide thickness. Of the four types of passivation treatment, the 400 °C thermal treatment exhibited the lowest content of suboxides and metallic elements and the thickest oxide by XPS analysis; however, this treatment may cause a desorption of the basic OH group in the hydration layer on the surface of titanium alloy.

Plasma spraying of zirconia-reinforced hydroxyapatite composite coatings on titanium: part II: dissolution behaviour in simulated body fluid and bonding degradation.

The change of phase, morphology and bond strength of plasma sprayed hydroxyapatite (HA) coating and ZrO2/HA composite coatings immersed in simulated body fluid (SBF) for various periods of time was studied. X-ray diffractometry (XRD) and scanning electron microscopy (SEM) were used to identify the phase and observe the morphology of the coating surface before and after immersion. In addition, inductively coupled plasma emission spectroscopy (ICP) was used to measure the ion release rate of coatings in SBF for various periods of time. Observation of the morphology by SEM shows that the composite coating with the addition of ZrO2 in HA significantly reduced the dissolution rate of impurity phases in simulated body fluid. The argument was supported by measurement of Ca2+ ion concentration in SBF. During plasma spraying, less OH- ions were lost in a ZrO2-containing composite coating. This factor, together with the reduced effective surface of the ZrO2-containing HA coating, were attributed to the reduced dissolution rate of the composite coatings. All the plasma sprayed coatings degraded after immersion in SBF owing to dissolution of constituents in the coating, however, the addition of ZrO2 in HA improved the bonding strength of HA coating after immersion in SBF.

Mechanical and histological evaluations of cobalt-chromium alloy and hydroxyapatite plasma-sprayed coatings in bone

This study evaluated the mechanical and histological behavior of cobalt-chromium (CoCr) alloy and hydroxyapatite (HA) plasma-sprayed coatings in canine cortical bone after 6 and 12 weeks of implantation, using CoCr alloy as the substrate. the substrate was bond-coated with microtextured CoCr alloy coating to ensure adherence between the substrate and top coats. A macrotextured CoCr alloy top coat with surface roughness Ra=34.25±5.50 μm was produced to create suitable pores ranging from 25 μm to 200 μm for bone ingrowth. For HA top coat, a relatively smooth surface (Ra=15.14±3.21 μm) was prepared for bone apposition. Shear testing of bone/implant interfaces showed that the CoCr alloy top coat exhibited significantly lower (p<0.01) mean shear strength than the HA top coat at each time interval. The maximum shear strength was 10.88±0.38 MPa for HA-coated implants 12 weeks post-implantation. After histological evaluations, substantial differences in the extent of new bone formation and the types of implant/bone contact were found between two kinds of implants. Direct bone-to-HA coating contact was consistently observed, while a layer of fibrous tissue intervening at the bone-CoCr alloy coating interface was found. Occasionally, partial dissolution of HA coating was seen after 12 weeks of implantation. The results of this study suggested that plasma-sprayed macrotextured CoCr coatings may not be an effective alternative for biological fixation.

Effect of passivation on the dissolution behavior of Ti6A14V and vacuum-brazed Ti6A14V in Hank's ethylene diamine tetra-acetic acid solution Part I Ion release

This work aims to investigate the effects of three factors, namely: (1) two differently prepared materials (as-polished Ti6A14V and 2 h brazed Ti6A14V); (2) three different surface passivation treatments (34% nitric acid passivation, 400°C heated in air, and aged in 100°C de-ionized water); and (3) periods of immersion time (up to 32 days), on trace element release in Hanks ethylene diamine tetra-acetic acid (EDTA) solution. After passivation and autoclaving treatment, the specimens were immersed in 8.0 mM EDTA in Hanks solution and maintained at 37°C for periods of time up to 32 days. The 400°C -treated specimens exhibit a substantial reduction in constituent release, which may be attributed to the higher thickness and rutile structure of the surface oxides. For acid-passivated and water-aged treatments, a highly significant decrease in the trace levels of Ti, A1, and V is detected from the brazed Ti6A14V compared to those obtained from the Ti6A14V specimens. It is hypothesized that an anatase–rutile transformation of surface TiO2 is likely to occur, accelerated by the elements of copper and nickel in the brazed specimens. In addition, a significant time-related decrease in constituent release rate is observed for all kinds of specimens throughout the 0–8 day experimental period. The implication of the results is discussed.

A comparison of the corrosion behaviour and surface characteristics of vacuum-brazed and heat-treated Ti6Al4V alloy

The corrosion characteristics of the brazed Ti6Al4V specimens were analysed and compared with respect to the conventionally heat-treated specimens by an electrochemical corrosion test. The object of this research was to explore the potentiality of the brazed titanium for biomaterials. The characteristics of the 1300 °C heat-treated and the 970 °C brazed specimens, with passivation and sterilization treatment, were evaluated by measurement of corrosion potential, Ecorr, corrosion current densities, Icorr, polarization resistance of the reacted surface films, Rp, in a potentiodynamic test. The experimental results show that the corrosion rates of the heat-treated and the brazed samples are similar at Ecorr, and the value of Ecorr for the brazed sample is noble to the heat-treated samples. The passive current density of the brazed specimen is either lower or higher than the heat-treated specimen, depending on the polarization potential. By Auger electron spectroscopic and high-resolution X-ray photoelectron spectroscopic analysis on specimens from the potentiostatic test, the elements of copper and nickel in the brazing filler were not detected while less alumina was found in the reacted film of the brazed specimens when compared with the heat-treated specimens. The implication of the results is discussed.