Enhancement of Wear and Corrosion Resistance of Beta Titanium Alloy by Laser Gas Alloying with Nitrogen

The relatively high elastic modulus coupled with the presence of toxic vanadium (V) in Ti6Al4 V alloy has long been a concern in orthopaedic applications. To solve the problem, a variety of non-toxic and low modulus beta-titanium (beta-Ti) alloys have been developed. Among the beta-Ti alloy family, the quaternary Ti-Nb-Zr-Ta (TNZT) alloys have received the highest attention as a promising replacement for Ti6Al4 V due to their lower elastic modulus and outstanding long term stability against corrosion in biological environments. However, the inferior wear resistance of TNZT is still a problem that must be resolved before commercialising in the orthopaedic market. In this work, a newly-developed laser surface treatment technique was employed to improve the surface properties of Ti-35.3Nb-7.3Zr-5.7Ta alloy. The surface structure and composition of the laser-treated TNZT surface were examined by grazing incidence x-ray diffraction (GI-XRD) and x-ray photoelectron spectroscopy (XPS). The wear and corrosion resistance were evaluated by pin-on-plate sliding test and anodic polarisation test in Hanks’ solution. The experimental results were compared with the untreated (or base) TNZT material. The research findings showed that the laser surface treatment technique reported in this work can effectively improve the wear and corrosion resistance of TNZT.

Corrosion behavior of pure titanium in artificial saliva solution

The biocompatibility of commercially pure (cp) titanium stems from its chemical stability within an organism, due to a fine film of impermeable titanium oxide covering the metal surface, which guarantees its resistance to corrosion. Despite its biocompatible characteristic, this material does not promote the formation of a hydroxyapatite layer, therefore, many research groups have sought to alter the material`s surface, introducing modifications that might influence corrosion resistance. The electrochemical behavior of cp Ti, with hydroxyapatite coating and without hydroxyapatite coating, commonly used in implant materials, was investigated using an artificial saliva solution at 25 degrees C and pH=7.4. In the conditions of the study it was observed that the hydroxyapatite layer influences the properties of corrosion resistance. This study of the behavior of cp Ti with and without hydroxyapatite coating, in naturally aerated artificial saliva solution at 25 degrees C, was based on open circuit potential measurements and potentiodynamic polarization curves. At approximately 1x10(-6) A/cm(2) the potential for cp Ti with and without hydroxyapatite coating begins to increase at a faster rate, but at -74mV (SCE) for coated cp Ti and at 180mV (SCE) for uncoated cp Ti the increase in potential begins to slow. This behavior, characterized by a partial stabilization of current density, indicates that in those potential ranges a protective passive film is formed.

Oxygen diffusion in Ti-10Mo alloys measured by mechanical spectroscopy

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Mechanical, physical, and chemical characterization of Ti-35Nb-5Zr and Ti-35Nb-10Zr casting alloys

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Evaluation of interface characterization and adhesion of glass ceramics to commercially pure titanium and gold alloy after thermal- and mechanical-loading

Objectives. This study evaluated the effect of thermal- and mechanical-cycling on the shear bond strength of three low-fusing glassy matrix dental ceramics to commercial pure titanium (cpTi) when compared to conventional feldspathic ceramic fused to gold alloy.Methods. Metallic frameworks (diameter: 5 min, thickness: 4 mm) (N = 96, n = 12 per group) were cast in cpTi and gold alloy, airborne particle abraded with 150 mu m aluminum oxide. Low-fusing glassy matrix ceramics and a conventional feldspathic ceramic were fired onto the alloys (thickness: 4mm). Four experimental groups were formed; Gr1 (control group): Vita Omega 900-Au-Pd alloy; Gr2: Ticeram-cpTi; Gr3: Super Porcelain Ti-22-cpTi and G4: Vita Titankeramik-cpTi. While half of the specimens from each ceramic-metal combination were randomly tested without aging (water storage at 37 C for 24h only), the other half were first thermocycled (6000 cycles, between 5 and 55 C, dwell time: 13 s) and then mechanically loaded (20,000 cycles under SON load, immersion in distilled water at 37 C). The ceramic-alloy interfaces were loaded under shear in a universal test machine (cross-head speed: 0.5 mm/min) until failure occur-red. Failure types were noted and the interfaces of the representative fractured specimens from each group were examined with stereo microscope and scanning electron microscope (SEM). in an additional study (N = 16, n = 2 per group), energy dispersive X-ray spectroscopy (EDS) analysis was performed from ceramic-alloy interfaces. Data were analyzed using ANOVA and Tukey's test.Results. Both ceramic-metal combinations (p < 0.001) and aging conditions (p < 0,001) significantly affected the mean bond strength values. Thermal- and mechanical-cycling decreased the bond strength (MPa) results significantly for Gr3 (33.4 +/- 4.2) and Gr4 (32.1 +/- 4.8) when compared to the non-aged groups (42.9 +/- 8.9, 42.4 +/- 5.2, respectively). Gr1 was not affected significantly from aging conditions (61.3 +/- 8.4 for control, 60.7 +/- 13.7 after aging) (p > 0.05). Stereomicroscope images showed exclusively adhesive failure types at the opaque ceramic-cpTi interfacial zone with no presence of ceramic on the substrate surface but with a visible dark titanium oxide layer in Groups 2-4 except Gr1 where remnants of bonder ceramic was visible. EDS analysis from the interfacial zone for cpTi-ceramic groups showed predominantly 34.5-85.1% O(2) followed by 1.1-36.7% Aland 0-36.3% Si except for Super Porcelain Ti-22 where a small quantity of Ba (1.4-8.3%), S (0.7%) and Sn (35.3%) was found. In the Au-Pd alloy-ceramic interface, 56.4-69.9% O(2) followed by 15.6-26.2% Si, 3.9-10.9% K, 2.8-6% Na, 4.4-9.6% Al and 0-0.04% Mg was observed.Significance. After thermal-cycling for 6000 times and mechanical-cycling for 20,000 times, Triceram-cpTi combination presented the least decrease among other ceramic-alloy combinations when compared to the mean bond strength results with Au-Pd alloy-Vita Omega 900 combination. (c) 2008 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Stress-induced ordering due heavy interstitial atoms in Nb-0.3 wt.% Ti alloys

The mechanical properties of metals with bee structure, such as niobium and their alloys, are changed of a significant way by the introduction of heavy interstitial elements. These interstitial elements (oxygen, for example) present in the metallic matrix occupy octahedral sites and constitute an elastic dipole of tetragonal symmetry and might produce anelastic relaxation. Polycrystalline samples of Nb-0.3 wt.% Ti (Nb-Ti) alloy with oxygen in solid solution were analysed. The anelastic spectroscopy measurements had been made in a torsion pendulum, with frequencies in the Hz range, in a temperature range between 300 and 700 K. The results showed thermally activated relaxation structures were identified four relaxation process attributed to stress-induced ordering of single oxygen, nitrogen and carbon atoms around niobium and stress-induced ordering of single oxygen atoms around titanium atoms. (c) 2005 Elsevier B.V. All rights reserved.

Vickers hardness of cast commercially pure titanium and Ti-6Al-4V alloy submitted to heat treatments

The purpose of this study was to evaluate the effect of heat treatments on the Vickers hardness of commercially pure titanium and Ti-6Al-4V cast alloys. Six-millimeter-diameter cylindrical specimens were cast in a Rematitan System. Commercially pure titanium and Ti-6Al-4V alloy specimens were randomly assigned to 3 groups (n=10) that received the following heat treatments: control (no heat treatment); treatment 1 (T1): heating at 750°C for 2 h; and treatment 2 (T2): annealing at 955°C for 1 h and aging at 620°C for 2 h. After heat treatments, the specimens were embedded in acrylic resin and their surface was ground and polished and hardness was measured. Vickers hardness means (VHN) and standard deviations were analyzed statistically by Kruskal-Wallis test at 5% significance level. For commercially pure titanium, Vickers hardness means of group T2 (259.90 VHN) was significantly higher than those of the other groups (control - 200.26 VHN and T1 - 202.23 VHN), which presented similar hardness means to each other (p>0.05). For Ti-6Al-4V alloy, statistically significant differences were observed among the three groups: T2 (369.08 VHN), T1 (351.94 VHN) and control (340.51 VHN) (p<0.05). The results demonstrated different hardness of CP Ti and Ti-6Al-4V when different heat treatments were used. For CP Ti, VHN means of T2 group was remarkably higher than those of control and T1 group, which showed similar VHN means to each other. For Ti-6Al-4V alloy, however, VHN means recorded for each group may be presented as follows: T2>T1>control.

Internal adaptation of cast titanium crowns

As the adaptation of titanium crowns obtained by Rematitan Plus investment, specific for titanium, is not recognized to be suitable, this study evaluated the effect of the concentration of the specific liquid and the temperature of the mold of investments on the internal misfit of crowns cast on commercially pure titanium. Individual dies of epoxy resin were obtained, representing teeth prepared for full-crown restoration with a 6-degree axial surface convergence angle and shoulder (1.0 mm). For the waxing of each crown, a ring-shaped stainless steel matrix (8.0mm internal diameter; 7.5 mm height) was adapted above the individual dies of epoxy resin. The Rematian Plus investment was mixed according to the manufacturer's instructions using two different concentrations of the specific liquid: 100%, 75%. Casting was performed in a Discovery Plasma Ar-arc vacuum-pressure casting machine with molds at temperatures of 430°C, 515°C and 600°C. The crowns were cleaned individually in a solution (1% HF + 13% HNO3) for 10 min using a ultrasonic cleaner, with no internal adaptations, and luted with zinc phosphate cement under a 5 kg static load. The crown and die assemblies were embedded in resin and sectioned longitudinally. The area occupied by cement was observed using stereoscopic lens (10X) and measured by the Leica Qwin image analysis system (mm2). The data for each experimental condition (n=8) were analyzed by Kruskal-Wallis non-parametric test (á=0.05). The results showed that liquid dilution and the increase in mold temperature did not significantly influence the levels of internal fit of the cast titanium crowns. The lowest means (±SD) of internal misfit were obtained for the 430°C/100%: (7.25 mm2 ±1.59) and 600°C/100% (8.8 mm2 ±2.25) groups, which presented statistically similar levels of internal misfit.

Effect of phosphate-bonded investments on titanium reaction layer and crown fit

This study analyzed the reaction layer and measured the marginal crown fit of cast titanium applied to different phosphate-bonded investments, prepared under the following conditions (liquid concentration/casting temperature): Rema Exakt (RE) - 100%/237°C, 75%/287°C, Castorit Super C (CS)-100%/70°C, 75%/141°C and Rematitan Plus (RP)-100%/430°C (special to titanium cast, as the control group). The reaction layer was studied using the Vickers hardness test, and analyzed by two way ANOVA and Tukey's HSD tests (α = 0.05). Digital photographs were taken of the crowns seated on the die, the misfit was measured using an image analysis system and One-way ANOVA, and Tukey's test was applied (α = 0.05). The hardness decreased from the surface (601.17 VHN) to 150 μm (204.03 VHN). The group CS 75%/141°C presented higher hardness than the other groups, revealing higher surface contamination, but there were no differences among the groups at measurements deeper than 150 μm. The castings made with CS - 100%/70°C presented the lowest levels of marginal misfit, followed by RE -100%/237°C. The conventional investments CS (100%) and RE (100%) showed better marginal fit than RP, but the CS (75%) had higher surface contamination.

Retention strength of cobalt-chromium vs nickel-chromium titanium vs Cp titanium in a cast framework association of removable partial overdenture

Aim: There is little information considering the framework association between cast clasps and attachments. The aim of this study was to evaluate the retention strength of frameworks match circumferential clasps and extra resilient attachment cast in three different alloys (cobalt-chromium, nickel-chromium titanium and commercially pure titanium), using two undercut (0.25 and 0.75 mm) and considering different period of time (0, 1/2, 1, 2, 3, 4 and 5 years). Methods: Using two metallic matrices, representing a partially edentulous mandibular right hemiarch with the first molar crown, canine root and without premolars, 60 frameworks were fabricated. Three groups (n = 20) of each metal were cast and each group was divided into two subgroups (n = 10), corresponding the molar undercut of 0.25 mm and 0.75 mm. The nylon male was positioned at the matrix and attached to the acrylic resin of the prosthetic base. The samples were subjected to an insertion and removal test under artificial saliva environment. Results: The data were analyzed and compared with ANOVAs and Tukey's test at 95% of probability. The groups cast in cobaltchromium and nickel-chromium-titanium had the highest mean retention strength (5.58 N and 6.36 N respectively) without significant difference between them, but statistically different from the group cast in commercially pure titanium, which had the lowest mean retention strength in all the periods (3.46 N). The association frameworks using nickel-chromium-titanium and cobalt-chromium could be used with 0.25 mm and 0.75 mm of undercut, but the titanium samples seems to decrease the retention strength, mainly in the 0.75 mm undercut. The circumferential clasps cast in commercially pure titanium used in 0.75 mm undercuts have a potential risk of fractures, especially after the 2nd year of use. Conclusion: This in vitro study showed that the framework association between cast clasp and an extra resilient attachment are suitable to the three metals evaluated, but strongly suggest extra care with commercially pure titanium in undercut of 0.75 mm. Clinical significance: Frameworks fabricated in Cp Ti tend to decrease in retentive strength over time and have a potential risk of fracture in less than 0.75 mm of undercut.

Flexibility and torsional resistance of three nickel-titanium retreatment instrument systems

Aim To assess the dimensional characteristics, flexibility and torsional behaviour of nickel-titanium retreatment instruments. Methodology Using image analysis software and high-resolution digital images, the instrument length, tip angle, diameter at 3mm from the tip and the distance between the blades (pitch length) of the following eight instruments were measured (n=12 for each measurement parameter): the ProTaper Universal retreatment (PTU-R) D1, D2 and D3 instruments; the R-Endo R1, R2 and R3 retreatment instruments; and the Mtwo retreatment (Mtwo-R) sizes 25 and 15 retreatment instruments. Maximum torque and the angular deflection at fracture as well as the bending moment at 45° were measured (n=12) according to the International Standards Organisation (ISO) specification number 3630-1. Data were analysed using the analysis of variance (α=0.05). Results The length of the active part of the instruments was found to vary according to the depth of the canal into which they were designed to reach. The pitch length also increased along the active length. The PTU-R D1 and the Mtwo-R instruments had active tips. Measurements of the bending moment at 45° revealed that the Mtwo-R 15 instrument was the most flexible, whereas the PTU-R D1 was the least flexible. The maximum torque tended to increase as the instrument diameter at 3mm from the tip increased, whereas the angular deflection at fracture varied in the opposite direction. Conclusions The geometrical characteristics of the retreatment instruments and their flexibility and torsion behaviour were consistent with their intended clinical application. © 2011 International Endodontic Journal.

Interstitial oxygen's influence on the corrosion behavior of Ti-9Mo alloys

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Tribocorrosion response of the Ti6Al4V alloys commonly used in femoral stems

In prosthesis, tribochemical reactions occur at the stem/bone interface. When coupled with micromotions it can lead to the loosening of the implant, osteolysis, release of metal ion and wear particles. The effect of these movements and the underlying mechanisms are quite unknown. This work investigates the tribocorrosion behavior of etched Ti6Al4V alloys under reciprocating sliding. Tests were performed in a phosphate buffer solution (PBS) containing proteins. A normal load of 1 N and anodic potentials of -0.1 and +0.5 V/SCE were applied. The destruction pathways of the top surface layers (adsorbed proteins, passive film) were studied. The results showed that the favorable/undesired effect of proteins in solution depends on the characteristics of the passive film under a mechanical stress. (C) 2013 Elsevier Ltd. All rights reserved.

A Quality Assessment of Titanium Castings Produced in an Experimental Short-Heating-Cycle Investment

The aim of this study was to evaluate the quality of casting produced in an experimental short-term heating-cycle investment. Thus, reaction layer and castability of titanium casting using an experimental spinel-based investment (VR) with short heating cycle were compared with the commercial short-heating-cycle spinel-based investment Trinell (TR), the silica-phosphate-based investment Rematitan Plus ( RP), and the conventional spinel-based investment Rematitan Ultra (RU). VR has polymeric fibers added to inorganic particles. Reaction layer assessments were carried out using Vickers hardness and elemental analysis using dispersive X-ray microanalysis (EDX). Mesh patterns were used for castability test, and powder characterization was made by scanning electron microscopy (SEM). Hardness evaluation showed no difference among the investments between 100 and 200 mu m. The most important contaminant element for VR, TR, and RU was oxygen. Higher levels of mold filling were found for TR, VR, and RU compared with that obtained with RP. The quality of castings, characterized by means of the assessments of reaction layer and castability, made from the VR was similar to the commercial investments TR and RU but superior to the RP.

Adhesive bonding of resin composite to various titanium surfaces using diferente metal conditioners and a surface modification system

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)