Nilson T. C. Oliveira

Studies on the stability of anodic oxides on zirconium biocompatible alloys

Studies on the stability of anodic oxides grown on zirconium and its biocompatible alloys Ti-50Zr at.% and Zr-2.5Nb wt.%, in aerated Ringer physiological solution, at 25 and 37 °C, were carried out by comparing their formation charge and their reconstruction charge after dissolution at open circuit in the physiological solution. The stability of oxides grown in the Ringer solution and in a 0.15 mol L-1 Na2SO4 solution was compared. The obtained results show that the stability of these oxides is increased by aging under potentiostatic conditions and can be decreased by the presence of chloride ions in the electrolyte during the anodization process.

Effect of an amorphous titania nanotubes coating on the fatigue and corrosion behaviors of the biomedical Ti-6Al-4V and Ti-6Al-7Nb alloys

An array of self-organized TiO2 nanotubes with an amorphous structure was produced on the biomedical Ti-6Al-4V and Ti-6Al-7Nb alloys, and the resulting fatigue and corrosion behaviors were studied. The electrochemical response of the nanotubular oxide surfaces was investigated in Ringer physiological solution through potentiodynamic polarization and electrochemical impedance spectroscopy measurements. The absence of transpassivation in the chloride-containing solution, in addition to the micron-scale values of the passivation current density, indicated the excellent corrosion behavior of the coating and the satisfactory protection against the creation of potential stress concentrators in the surface. Axial fatigue tests were performed in physiological solution on polished and coated conditions, with characterization of the treated surfaces by scanning electron microscopy before and after the tests. The surface modification was not deleterious to the fatigue response of both alloys mainly due to the nano-scale dimension of the nanotubes layer. An estimation based on fracture mechanics revealed that a circumferential crack in the range of 5μm depth would be necessary to affect the fatigue performance, which is far from the thickness of the studied coating, although no cracks were actually observed in the oxide surfaces after the tests.

Bioactivity of self-organized TiO2 nanotubes used as surface treatment on Ti biomaterials

Titanium and its alloys are widely used as implants due to their excellent mechanical properties, corrosion resistance and biocompatibility. TiO2 nanotubes have been studied as surface treatment to increase the specific area and to improve osseointegration. However, the thermodynamic stability and bioactivity of these nanostructures must be evaluated. The objective of this research was to obtain nanotubes oxides on Ti6Al4V alloy and to analyze the electrochemical stability in physiological solution at 37 °C and the bioactive response of the biomaterial. The nanotubes were obtained by potentiostatic anodization. The morphology of the oxides was evaluated by scanning electron microscopy. The chemical characterization was analyzed by energy dispersive spectroscopy and x-ray photoelectron spectroscopy techniques. The electrochemical stability was analyzed by open circuit potential (OCP) and the bioactivity by biomimetic test in a simulated body fluid (SBF) solution. The OCP of the nanotubes oxides was shown to be more noble and stable than the compacted oxides. The biomaterial covered with theses oxides showed sealing by Ca and P after 30 d immersion in artificial blood. And after 15 d of immersion in SBF, the hydroxyapatite could be seen on the non-sealed nanotubes. TiO2 nanotube layers could improve the superficial chemical stability and also the osseointegration process.

Elastic modulus evaluation of Titania nanotubes obtained by anodic oxidation

The use of titania (TiO2) nanotubes is becoming one of the most attractive techniques as surface treatment for implants due its combination of morphology (that accelerates osteoblast adhesion and proliferation), bioactivity and possibility of being use as a drug vehicle. Anodic oxidation is one of the cheapest and simplest approaches to obtain highly ordered nanotubes. Parameters such as applied potential, reaction time and fluoride containing in the electrolyte define the nanotubes morphology. However, the mechanical properties of the nanotubes layer do not have been completely elucidated and they play a crucial role in the implant long term stability. The objective of this research was to obtain TiO2nanotubes using anodic oxidation and to determine their elastic modulus and hardness. The TiO2nanotubes layer was obtained in a fluoride containing electrolyte for 1 hour, one group at 15 V and another one at 25 V. The TiO2nanotubes morphology was characterized by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The elastic modulus and hardness were evaluated by nanoindentation experiments using a spherical tip. SEM images showed highly ordered nanotubes on all titanium surfaces and it was observed that the nanotubes diameters are directly related with the applied potential. Nanotubes diameters are 66 ± 9 nm and 131 ± 22 nm for nanotubes obtained at 15 V and 25 V, respectively. Nanoindentation test results showed a decrease in the elastic modulus comparing with titanium reference and these values approach to cortical bone elastic modulus. These results demonstrate that it was possible to obtain a homogeneous TiO2nanotubes layer that has mechanical properties adequate to improve implant long-term stability.

Growth and electrochemical stability of self-organized TiO2nanotubes on Ti-2 grade and orthopedic Ti6Al4V alloy for biomedical application

Titanium and its alloys are biomaterials used in endosseous implants, due to desirable mechanical properties, high corrosion resistance and biocompatibility. Using electrochemical anodization technique these materials can be recovered with self-organized TiO2 nanotubes layer resulting in increased specific surface area and probable bioactivity improvement. This research aimed determine potentiostatic anodization parameters to obtain self-organized TiO2nanotubes layer with reproducibility and ideal diameters for probable bioactive response on Ti - 2 grade (ASTM F67) and Ti6Al4V (ASTM F136) orthopedic alloy and evaluation the electrochemical stability behavior in simulated body fluid media. The self-organized nanotubes layer were obtained by potentiostatic electrochemical method in electrolyte containing fluoride ions, H3PO4/HF for Ti 2 grade and H3PO4/NH4F for Ti6Al4V alloy, the applied potentials were 15 V, 20 V and 25 V for 30, 60 and 90 minutes, for both materials. For morphologic characterization were employed scanning electron microscopy SEM and the Image J software for nanodiameter measurements. The nanoestructure electrochemical stability was evaluated by open circuit potential after immersion for 15, 30 and 60 days in artificial blood plasma, into an electrochemical cell, using SCE (saturated calomel electrode) as reference electrode, in PBS ((phosphate buffered saline) solution electrolyte for 90 minutes. The ideal anodization parameters were 15 V and 20 V for 1 hour and a reproducible, uniform and homogeneous self-organized nanotubes layer were obtained with ideal diameters that probably improve the implant superficial bioactivity with 80 and 120 nm respectively, according to the literature. Open-circuit potentials from metal/oxide system obtained on both materials are stable with potentials in range of -0.031 V to -0,183 V indicating good stability of nanoestructures in simulated body fluid. Nanotubes layer as a superficial treatment is viable with high reproducibility, low cost and electrochemical stability in simulated body fluid media.

Fatigue Performance of New Developed Biomedical Ti-15Mo Alloy with Surface Modified by TiO2 Nanotubes Formation

In recent years, it was demonstrated that Ti-Mo alloys are promising to be use as orthopedic implants. The presence of TiO2 nanotubes can increase the bioactivity and improve the osseointegration of Ti and its alloys implants, although this modification could lead to a reduction in the dynamic mechanical properties. In this context, the purpose of the present study was to obtain self-organized nanotubes on the surface of biomedical Ti-15Mo alloy and verify whether the fatigue performance was significantly changed. Organized nanotubes were obtained by anodic oxidation using ethylene glycol + NH4F solution. The axial fatigue behavior was characterized by stepwise increases of the applied load in air and in physiological media at 37°C. The results was compared with the as-polished samples in order to compare if the Ti-15Mo alloy fatigue behavior was affected by the surface modification, and it was found that the mechanical performance of the Ti-15Mo alloy was affected by the surface modification, in that specific experimental conditions used to obtain the nanotubes.