ABSTRACT 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.

The present study produced binary titanium-niobium alloys Ti-xNb with high niobium percentage (x = 50, 80 e 90 wt.%) aiming to apply it as a base material in osseous implant devices. The produced TiNb alloys presented a cubic crystalline phase, lower corrosion rate than titanium, lower elastic modulus values, and superior cellular viability than titanium and niobium. The Ti50Nb alloy among all analyzed metallic substrates showed the best values of elastic modulus, corrosion properties, wettability, and cellular viability. Thus, this work suggests a Ti/Nb ratio close to 1 (Ti50Nb) displays optimum characteristics to apply in orthopedic devices.

Neste trabalho são estudados os efeitos da adição de nanotubos de carbono de parede múltipla (NCPM) em uma matriz de Poli(L-ácido láctico) (PLLA). Foras avaliadas duas rotas distintas de dispersão dos NCPM, uma utilizando agitação mecânica em solvente e a outra utilizando sonificação de alta energia em solvente. As propriedades mecânicas destes nanocompósitos foram avaliadas utilizando nanoindentação e microdureza vickers. Através da calorimetria exploratória diferencial foram determinadas as propriedades térmicas dos nanocompósitos (Tg, Tc, Tm e cristalinidade) obtidas. Por último, as propriedades tribológicas foram determinadas através de ensaios de deslizamento do tipo pino sobre disco, onde foram utilizadas diferentes cargas normais. As propriedades mecânicas e térmicas não foram significativamente afetadas pela adição do nanotubos, o que não se repetiu nas propriedades tribológicas, onde tanto o método de dispersão quanto a concentração de NCPM afetaram as propriedades. A micrografia das trilhas de desgaste sugere ainda que o mecanismo atuante foi modificado com a incorporação dos nanotubos, o mesmo pode ter acontecido nas amostras sonificadas.

This work studied the effects of the addition of Multiwalled Carbon Nanotubes (MWCNT) to a PLLA matrix. Two distinct methods of preparation were employed: a combination of a solvent/ mechanical stirring and a combination of a solvent/high energy sonication. The mechanical properties of the nanocomposites were determined by nanoindentation and by the Vickers hardness test. Thermal properties of the nanocomposites (Tg, Tc, Tm and crystallinity degree) were determined by DSC. The tribological properties of the nanocomposites were determined by using a pin-on-disc apparatus. Mechanical and thermal properties did not present significant alterations, although tribological properties presented significant changes caused by the method of preparation and different loads. SEM images indicated that the wear mechanism was changed by the addition of MWCNT.

This work aims to characterize the phases, thickness, hardness and hardness profiles of the nitride layers formed on the CA-6NM martensitic stainless steel which was plasma nitrided in gas mixtures containing different nitrogen amounts. Nitriding was performed at 500 ºC temperature, and 532 Pa (4 Torr) pressure, for gas mixtures of 5% N2 + 95% H2, 10% N2 + 90% H2, and 20% N2 + 80% H2, and 2 hours nitriding time. A 6 hours nitriding time condition for gas mixture of 5% N2 + 95% H2 was also studied. Nitrided samples results were compared with non-nitrided condition. Thickness and microstructure of the nitrided layers were characterized by optical microscopy (OM), using Villela and Nital etchants, and the phases were identified by X-ray diffraction. Hardness profiles and hardness measured on surface steel were determined using Vickers hardness and nanoindentation tester, respectively. It was verified that nitrided layer produced in CA-6NM martensitc stainless steel is constituted of compound layer, being that formation of the diffusion zone was not observed for the studied conditions. The higher the nitrogen amounts in gas mixture the higher is the thickness of the nitrided layer and the probability to form different nitride phases, in the case γ'-Fe4N, ε-Fe2-3N and CrN phases. Intrinsic hardness of the nitrided layers produced in the CA-6NM stainless steel is about 12-14 GPa (~1200-1400 HV).

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.

RESUMO Esse trabalho apresenta um estudo da dureza e do mee austenita-γ da liga inoxidável à base de ferro com efeito de memória de forma. Utilizando indentação instrumentada, foi possível determinar a dureza e o módulo de elasticidade das fases austenita-γ e martensita-ε separadamente. A fase martensítica apresentou uma dureza de 7,0 GPa, enquanto que a dureza da fase austenítica foi de 3,0 GPa. Os valores de módulo de elasticidade foram 202 e 137 GPa, para as fases martensita e austenita, respectivamente.

ABSTRACT This work presents a hardness study and elastic modulus for the ε-martensite and γ-austenite phases of an iron based shape memory alloy. Using instrumented indentation, it was possible to determine the hardness and elasticity modulus of these phases separately. The martensitic phase presented a hardness of 7.0 GPa and the austenitic phase presented a hardness of 3.0 GPa. The elastic modulus values were 202 and 137 GPa for the martensitic and austenitic phases, respectively.

The effects of Ag addition on some physical properties of YBa2Cu3O7-δ superconductor has been studied. The samples were produced by different routes and characterized by scanning electron microscopy, differential thermal analysis, thermogravimetric analysis, X-ray diffraction and nanoindentation. The superconducting properties were studied by dc magnetization and electrical resistivity measurements. The X-ray patterns revealed that all samples were polycrystalline and corresponded to the orthorhombic YBa2Cu3O7-δ phase. However, for some samples, silver appears to be present within the grains. The superconducting properties were not significantly influenced by Ag addition. Hardness and elastic modulus were also obtained by instrumented indentation. Ag addition was found to be effective in improving the mechanical properties, probably by filling the pores in the grain boundaries. Hardness profiles indicated values between 3.1 and 3.4 GPa at deep tip penetration depths. The highest elastic modulus of 146 GPa was attained for samples prepared using Y2O3, BaCO3, CuO and Ag2O as precursors, while the lowest modulus (125 GPa) was obtained for the pure YBa2Cu3O7-δ sample.

The nanoindentation technique allows the determination of mechanical properties at nanometric scale. Hardness (H) and elastic modulus (E) profiles are usually determined by using the Oliver-Pharr method from the load/unload curves. This approach is valid only for flat surfaces, or at least, when a very low degree of asperity is present (lower than 30 nm). The basic statement is the determination of the zero tip-surface contact point. If a rough surface is present, errors can occur in determining this contact point and, as a consequence, the surface hardness and elastic modulus profiles are drastically altered resulting in under evaluated values. Surfaces with different roughness were produced by controlled nitrogen glow discharge process on titanium. The changed nitriding parameters were different N2/H2 atmospheres and temperatures (600 °C-900 °C). The most correct H and E profiles were obtained by using the contact stiffness analysis method, proposed here, that overcomes the surface roughness. The obtained results were compared with available literature data.

Based on the fact that the Ti-6Al-4V alloy has good mechanical properties, excellent resistance to corrosion and also excellent biocompatibility, however with low wear resistance, this work aims to test plasma processes or combination of plasma and ion implantation processes to improve these characteristics. Two types of processing were used: two steps PIII (Plasma Immersion Ion Implantation) combined with PN (Plasma Nitriding) and single step PIII treatment. According to Auger Electron Spectroscopy (AES) results, the best solution was obtained by PIII for 150 minutes resulting in ~ 65 nm of nitrogen implanted layer, while the sample treated with PIII (75 minutes) and PN (75 minutes) reached ~ 35 nm implanted layer. The improvement of surface properties could also be confirmed by the nanoindentation technique, with values of hardness increasing for both processes. AFM (Atomic Force Microscopy) characterization showed that the single step PIII process presented greater efficiency than the duplex process (PIII + PN), probably due to the sputtering occurring during the second step (PN) removing partially the implanted layer of first step (PIII).