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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.

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.

There are various surface treatments used to modify titanium surfaces to render it bioactive. In this study commercially pure titanium surfaces (cp Ti), grade 2 were modified by acid etching (AE) and anodic oxidation (OA) in order to evaluate the bioactivity in vitro of these surfaces using the simulated body fluid (SBF). The AE was realized using a mixture of acids and AO using 1 mol.L-1 sulfuric acid. The anodic films were obtained under potentiostatic mode, during 60s using as anode a bar of titanium. All the surfaces that means cp Ti, AE and AO were analyzed concerning to morphology, rugosity, structural changes before in vitro bioactivity tests. It was observed by scanning electron microscopy (SEM) that all surfaces presented different morphologies: those with AE showed a surface with peaks and rounded valleys, with Ra = (564±80) nm, the oxidized surfaces with sulfuric acid showed a morphology with small pores uniformly distributed over the surface and Ra = (177±0,02) nm. X-rays diffraction results showed the presence of titanium hydride on the samples with AE and the anatase and rutile phases on the anodic films after heat treatment at 600°C/1h. Bioactivity tests in vitro using SBF at 37°C showed that small aggregates containing Ca and P were observed on surfaces with AE after 30 days soaked in SBF and the surfaces oxidized were fully coated with an apatite layer, identified by SEM.

Nesse trabalho, apresentamos a caracterização estrutural de regiões soldadas em aço austenítico AISI-304, que foram submetidas a processo de nitretação a plasma (20%N2 + 80%H2). Posteriormente as amostras foram hidrogenadas catodicamente. As temperaturas de nitretação foram de 400, 500 e 550°C. As regiões da solda e fora da solda hidrogenadas após a nitretação foram comparadas por DRX, microscopia ótica e microscopia eletrônica de varredura (MEV). As fases austenita-γ, martensita-α', martensita-ε, ferrita-α e os nitretos CrN, γ'-Fe4N e e-Fe2+xN foram identificados. As microestruturas de ambas as regiões e da zona termicamente ativada (ZTA) foram similares. Para 400°C, a estequiometria das fases formadas foi diferente das observadas em 500°C e 550°C. Os efeitos provocados pela hidrogenação foram mais acentuados em 550°C, com o arrancamento da camada nitretada. Structural characterization of weld and outside weld regions of AISI-304 nitrided (20%N + 80%H) and cathodically hydrogenated is presented. Nitriding temperatures were 400, 500 e 550°C. The weld and outside weld regions were compared by XRD, optical microscopy and SEM. The phases γ-austenite, α'-martensite, ε-martensita and α-ferrite and the nitrides: CrN, γ'-Fe4N e e-Fe2+xN were identified. Microstructures of both regions and the thermal active zone were similar. For 400°C the stoichiometry of the formed phases was different from that formed at 500°C and 550°C. Hydrogen effects were more intense for 550°C, due to chipping occurrence.

Osteoblast adhesion on metallic titanium coated with anodic films was evaluated. The anodic oxidation treatment was carried out on commercially pure-titanium (cp-Ti) substrate under the following conditions: 1.0M H2SO4/150V and 1.0M Na2SO4/100V. Osteoblast cells were cultured onto the samples for 4 hours. The morphologies of both Ti anodic films and cells were observed by scanning electron microscopy (SEM). The oxide films are rough with porous structure. Statistical differences in average surface roughness (Ra) values are found among both anodic films and substrate (abraded cp-Ti), measured by contact profilometry. The oxide films prepared in H2SO4 had greater contact angle, whereas there is no statistical significance between the values for the Ti anodic films produced in Na2SO4 and the substrate surface. Despite the some differences in morphology, roughness and contact angle between the treated and non-treated samples, cell morphologies were similar on all surfaces after 4h of culture. Further, was not clearly observed a correlation between the surface characteristics with cell behavior.