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Due to the advances in surface treatments, it is possible to obtain excellent cutting tools. However, the field for wood cutting tools still needs to be further investigated. In this work, titanium nitride was deposited on bandsaw blades by the cold plasma technique to increase the lifespan of the wood cutting tool, improving the coated surface. Tests were performed by varying the conditions in the amount of nitrogen and time. In addition, the industrial physical vapor deposition technique was also performed as a comparison. The morphology, structural changes and chemical mapping of the coated samples were investigated with a focus on their mechanical properties by nanoindentation and tribology tests. The surfaces were coated uniformly, with a well-adhered TiNx layer identified by X-ray diffraction and Raman spectroscopy and the electron-dispersive X-ray spectroscopy technique, it was possible to identify the presence of nitrogen in all deposited films. Although no significant differences were observed in hardness values for cold-plasma treated surfaces compared to the uncoated, their friction coefficients and wear values were lower. Physical vapor deposition coated samples had the lowest friction coefficient and wear values. In field trials, the coated cold plasma bandsaw blades had the lowest deviation when cutting the wood and show that this technique can be used for this purpose. yes

Among titanium alloys with non-toxic elements, the Ti-25Nb-25Ta alloy has good elastic behavior for applications in osseous implants, biocompatibility, and excellent corrosion resistance. The present study aimed to better the biocompatibility characteristics of Ti-25Nb-25Ta alloy modifying its surface through Plasma Electrolytic Oxidation (PEO) treatment. The formed oxide coating is amorphous and composed of two distinct porous formations: smaller hole-shaped pores and larger volcano-like pores. The regions with the formation of smaller pores and in the hole shaped presented the highest atomic percentage of the chemical element phosphorus. Nanoindentation tests have shown that the hardness of the Ti-25Nb-25Ta alloy is slightly lower than the commercially pure grade 2 titanium (a material used as reference), while elastic modulus measurements of Ti-25Nb-25Ta presented more suitable values for implant application (lower values when compared with titanium reference). After PEO treatment there were significant mechanical surface improvements (increased fairly surface hardness and decreased elastic modulus) for application in osseous tissue. Despite the Ti-25Nb-25Ta alloy presented excellent characteristics for applications in hard biological tissues, the PEO treatment better its features. Keywords: Titanium alloy, Ti-25Nb-25Ta, nanoindentation, mechanical properties, Plasma Electrolytic Oxidation.

Well-adhered nanotube arrays were produced through the anodizing technique on a Ti-25Nb-25Ta alloy and tribo-mechanically evaluated by nanoindentation and nanoscratch tests. Disregarding substrate effects, the hardness of the nanotube arrays layer was 0.7 ± 0.1 GPa and elastic modulus was

International audience; Surface modification by deposition of hard coatings is a way to overpass the poor wear resistance of some metallic materials and one potential material is the Diamond-Like Carbon (DLC). We investigated the wear behavior, and the adhesion of the DLC deposited on a Ti6Al4V (Ti64) alloy after Surface Mechanical Attrition Treatment (SMAT). The SMAT was applied using 100Cr6 steel balls, and the DLC was deposited through the sputtering method. The nano-hardness was evaluated using a MTS Nano Indenter XP. The adhesion of the DLC was evaluated using a CSM Revetest, and the wear tests was performed in a reciprocating linear tribometer from CSM Instruments. The mean wear rate for the Ti64 was 437x10-6 mm3/N/m against 5x10-6 mm3/N/m for the Ti64+SMAT+DLC. The SMAT reduced the wear rate of the DLC coating, showing that the SMAT might be a viable treatment with promising results regarding the DLC wear resistance.

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.

In this work, the resistance to scratch and wear (pin-on-flat) tests of five different porous TiO2 films were compared. Such tribological tests were carried out under dry conditions. The coatings were electrodeposited on commercially pure-Ti by anodic oxidation method in different electrolyte solutions at constant voltages. The scratch tests were conducted by applying increasing normal loads up to 400 mN. The coefficient of friction (COF) varied from 0.2 up to 0.5, and increased at larger penetrations depths. When the electrolyte concentration was changed from 0.5 into 1.0M H2SO4, the COF slightly decreased. Scanning electron microscopy indicated that the coatings produced in H2SO4/150V and Na2SO4/100V did not have their substrates revealed. In addition, the samples anodized in H2SO4/150V had the highest elastic recoveries. Therefore, such coatings seem to be more resistant to scratch tests than the others. The wear tests were carried out with Berkovich tip as counter-face under constant normal loads of 10 mN in 10 forward-backward cycles. The coatings deposited in H2SO4/150V had the lowest wear volume rates. The findings suggest that the porous Ti oxide coatings electrodeposited above their rupture voltages are more suitable to both scratch- and wear-resistance compared to those prepared at the lowest voltage (H2SO4/100V).

Titanium has been used in the production of dental implants and orthopedic prostheses due to the low tendency to corrosion and good biocompatibility. Meanwhile, the surface of titanium is not bioactive. Several surface treatments have been developed to make the surface of such metals bioactive. The aim of this work was to evaluate two of these modification processes in commercially pure titanium grade 2, both of them using NaOH solutions: the anodic oxidation and the alkali treatment. The surface morphology was evaluated by SEM/EDS, the crystal structure by XRD, and the mechanical properties and scratch resistance by instrumented indentation. The anodic oxidation (AO) was carried out using NaOH electrolyte 0.1 mol/L and constant current density of 150 mA/cm² for one minute. The alkaline treatment (AT) was performed by soaking the Ti sample in NaOH 5 mol/L solution at 60 °C for 24 hours; after this, the sample was heat treated at 600 °C for one hour in atmospheric air. The AO produced a TiO2 layer on Ti, whereas a thin sodium titanate layer was obtained by AT. Each surface modification resulted in a specific morphology, but both of them presented the increase in roughness as a common characteristic. The alkali treated Ti surfaces showed the lowest elastic modulus and hardness values. The largest increase in hardness between the treated surfaces was obtained for Ti after anodic oxidation. Scratch test indicates that the TiO2 film from AO has higher strength to tangential loading than the Ti substrate. In addition, for the Ti submitted to AT, the scratch test indicates that the modified surface layer has a poor adhesion with the substrate. Based on these results it is possible to conclude that, using NaOH solutions, Ti surfaces treated by anodic oxidation present improved mechanical properties than the alkali-treated ones.

Hydrogen diffusion is a well-known cause of embrittlement in titanium devices, however the use of H-implantation has been investigated to enhance the titanium biocompatibility and bioactivity. In the present study, effects of the hydrogen ion implantation on Ti and nitrided Ti through glow discharge are reported, focusing the surface tribo-mechanical response at nanoscale. The structural and chemical features were also evaluated, before and after the hydrogen implantation, by NRA, XRD, XPS, SEM and EDS. The hydrogen implantation increased the H content on Ti up to two times, promoted the formation of δ-TiH precipitates and changed the Ti oxidation state, without affecting hardness and elastic modulus. Hydrogen implanted after nitriding produced blisters, formed by H accumulation near the surface region of the nitride layer due to its barrier effect. A “denitriding” process at very near surface region was also observed after the hydrogenation. Nitriding increased Ti hardness by 120% and elastic modulus by 18%. Hydrogenation became the nitrided Ti harder and stiffer, increasing the hardness and elastic modulus by 180% and 41%, respectively. In both Ti and nitrided Ti, nanotribological tests pointed out that the surface became brittle after hydrogenation. On the other hand, the H-implantation had negligible effects on the Ti and nitrided Ti tribological behaviors in the tests performed under severe dry conditions.

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.

Although titanium metal has been used intensively in the last years as biomaterial in the medical and dental areas its surface is not bioactive. In this work, titanium metal was submitted to an alkali treatment in order to make the metal surface bioactive. The samples were submitted to alkaline treatment (AT) using NaOH 5M aqueous solution at 60°C for 24 h and after that they were heated thermically to stabilize the layer obtained with AT. The bioactivity of the samples was evaluated soaking them into the simulated body fluid (SBF) at 36,5°C for 28 days. The morphological, structural changes and the electrochemical characterization were analyzed using scanning electron microscopy, x-ray diffraction and electrochemical impedance spectroscopy (EIS), respectively. It was verified that after AT plus heat treatment (HT) a sodium titanate layer was formed on the samples surface and after the bioactivity tests an apatite layer was formed. Impedance analysis show that the resistance of film on Ti is high and this value increases when the sample is soaked in SBF. It means that the apatite (HPA) film is occurring and the value of the capacitance with the presence of the HPA film (Cp) values indicate that the film maintain a compact and uniform characteristics.

Anodic oxidation is a promising technique to become titanium surfaces bioactive, by simultaneously changing the surface morphology, structure and chemical properties. Calcium and phosphorus based electrolytes were used to produce anodic films on c.p. Ti with two different current densities, 150 mA/cm2 and 300 mA/cm2. Morphology and structure were examined by SEM, EDS and XRD, and elastic modulus and hardness of the surfaces by instrumented indentation. Besides rutile and anatase TiO2 phases, hydroxyapatite was also identified on the films, as well as the segregation of very soft Ca and P-rich zones. Low values for the elastic modulus and hardness values close to the Ti corroborate to the applicability of Ca and P based TiO2 anodic films in biomedical titanium implants.

Two different Ti oxide films produced by anodic oxidation were submitted to in vitro bioactivity and cell culture tests. The oxide films were produced in 1.0M H2SO4/150V and 1.0M Na2SO4/100V. Surfaces were found to be homogeneous and rough, with the presence of pores. Both oxide films presented anatase and rutile phases. Ti oxide film produced in Na2SO4 was rougher than the film grown with H2SO4 and composed of a rutile-rich phase. Both films were constituted by TiO2 and Ti2O3 oxides. Despite the differences observed, after 7 days, a calcium phosphate layer was precipitated on both surfaces. Indeed, these two treatment conditions seem to be efficient to spread and attach osteoblast-like cells within 4h.

We evaluated the nano-hardness, elastic modulus and brittleness of titanium oxide (titania) films produced by anodic oxidation for biomedical applications. These mechanical properties were studied as a function of depth displacement with respect to electrolyte concentration and potential applied to the electrochemical treatment. The measurements were performed by instrumented indentation tests in air. For shallow depths, the nano-indentation results showed that the nano-hardness of the titania films were greater than those for commercially pure Ti (cp-Ti), and that they varied with the applied potential. Also the elastic modulus values were smaller as compared to those of cp-Ti, and they showed to be little influenced by electrolyte concentration and/or applied potential. Some impressions from the nano-indenter tip on the titania films were observed by scanning electron microscopy (SEM). Despite the promising results obtained, namely, hard films with reduced elastic modulus, the SEM images revealed some micro-cracks from indenter impressions in the oxide films produced in H2SO4 at 150 V. These results thus indicate that Ti anodic films on cp-Ti can be applied to the medical field when submitted to low loads (

Titanium oxide films produced on commercially pure Ti by anodic oxidation with different voltages were analyzed. Anodic oxidation was carried out at room temperature using 1.4 M H 3 PO 4 electrolyte and a platinum counter-electrode, in potentiostatic mode under the following conditions: 50 V, 100 V, 150 V, 200 V and 250 V. It was observed that porous titanium layers were formed at all voltage values but morphological differences were observed. Initially, the film was thin but with increasing voltage it broke down locally and porous regions became evident due to the dielectric breakdown. The porosity and the pore size increased with the increasing voltage. The surface morphology in samples formed with 200 V had substantially different porous structures than those formed with other voltage values. The anodic film surface displayed pores and craters formed on the relatively flat ground oxide surface. AFM images showed that higher voltages produced thicker titanium oxide films.

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.

Bone formation around a metallic implant is a complex process that involves micro- and nanometric interactions. Several surface treatments, including coatings were developed in order to obtain faster osseointegration. To understand the role of these surface treatments on bone formation it is necessary to choose adequate characterization techniques. Among them, we have selected electron microscopy, profilometry, atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS) to describe them briefly. Examples of the potentialities of these techniques on the characterization of titanium for biomedical applications were also presented and discussed. Unfortunately more than one technique is usually necessary to describe conveniently the topography (scanning electron microsocopy, profilometry and/or AFM) and the chemical state (XPS) of the external layer of the material surface. The employment of the techniques above described can be useful especially for the development of new materials or products.

Hydrogen effects in austenitic steels submitted to fatigue tests have been studied. Superficial H was introduced cathodically at 50 °C using 1N H2SO4 solution, a platinum counter electrode and a current density of 1000 A/m2 during 4 h. Internal H was introduced cathodically using a mixture of the salts KHSO4 and NaHSO4 at 200 °C during 60 h by applying a constant polarization potential of 850 mV with respect to a silver reference electrode. Fatigue tests were carried out by using a alternate flexion fatigue machine with stress ratio R values equal 1 and frequency of 50 Hz. The samples were tested until the fracture of the material was reached or until the stipulated fatigue limit life was reached. Results showed that superficial H introduced surface cracks during outgassing process while internal hydrogenation did not modify the superficial conditions. Mechanical tests showed that H reduced the fatigue life of these steels, and this effect was even more accentuated at lower stresses. Superficial hydrogenation presented inter and transgranular fracture and the morphology of the fracture remained ductile while internal H presented transgranular fracture and some regions with fracture by cleavage process.

Hydrogenation effects on the nanohardness of 304L/308L austenitic stainless steel joints have been studied. Surface cracks and α′ martensitic phase are nucleated during aging at room temperature (RT) and the nucleation kinetic depends on the hydrogen (H) outgassing time. Since these effects are confined on the superficial layers of the material, nanoindentation test is a powerful tool to analyze the region modified by H. The hydrogenation was performed cathodically at RT, during 4 h, using an electrolyte of 1 N H 2 SO 4 containing 100 mg l −1 of As 2 O 3 . A platinum counter electrode and a current density of 1000 A m −2 were used. In this work nanoindentation tests were performed as soon as the hydrogenation was interrupted and with the outgassing time varying up from hours to some days. It was observed that nanohardness have high values in the base and weld metal (WM) just after the hydrogenation process have been interrupted and that decreases with H outgassing time. After several days of outgassing time it was observed a significant decrease in hardness of base metal (BM) and WM when compared with a material without H.

Tritium autoradiography was used to study the tritium distribution in laser and arc (TIG) weldments performed on tritiated AISI 316 samples. Quantitative values of the local tritium concentration were obtained from the microdensitometric analysis of the autoradiographs. This procedure was used to map the tritium concentration in the samples before and after laser and TIG treatments. The effect of the detritiation conditions and of welding on the tritium distribution in the material is extensively characterized. The results illustrate the interest of the technique for predicting a possible embrittlement of the material associated with a local enhancement of the tritium concentration and the presence of helium 3 generated by tritium decay.