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.

Thermal stability of the martensitic transformation of Cu-Al-Ni-Mn-Ti

The development of new shape memory alloys with high martensitic transformation temperature increases the potential for applications. The development and use of these new alloys depends on the stability of the structure during cycling at high temperatures. If it is possible to guarantee that on alloys keeps the structure during cycling, then the alloy can be used because of the shape memory properties. The aim of this work is to obtain a kinetic model of the forward and backward martensitic transformation of two Cu-Al-Ni-Mn-Ti alloys. Differential scanning calorimetry has been performed in order to establish the kinetic stability of the martensite and the beta transformation. (c) 2006 Elsevier B.V. All rights reserved.

Estudo do biomaterial Ti-6Al-4V empregando-se técnicas eletroquímicas e XPS

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

Electrochemical stability and corrosion resistance of Ti-Mo alloys for biomedical applications

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

Internal friction measurements in Nb-0.3wt.%Ti containing oxygen

Internal friction measurements were made in the Nb-Ti alloy containing 0.3 wt. % of Ti, doped with various quantities of oxygen (0.04 to 0.08 wt. %) utilizing a torsion pendulum. These measurements were performed in the temperature range of 300 K to 700 K with the oscillation frequency about 1.0 Hz. The experimental results showed relaxation peaks due the stress induced ordering of oxygen atom and pairs of oxygen atom around the niobium atoms (metallic matrix) and around titanium atoms (substitutional solute).

The effect of mold temperature on castability of CPTi and Ti-6Al-4V castings into phosphate bonded investment materials

Objective. The aim of this study was to evaluate the castability of CP titanium and Ti-6Al-4V alloy castings into Rematitan Plus investment at three different mold temperatures.Methods. A nylon mesh pattern (20 mm with 64 squares and wire of 0.7 mm in diameter) was used for the castability testing. Initially, an image of the wax pattern was obtained by means of a digital camera and the total extension of filaments (mm) was then measured, using the Leica Qwin image analysis system. The mesh sprued was placed in the Rematitan Plus investment material and the castings were made in a Discovery Plasma machine at three different mold temperatures: 430 degrees C (control group), 480 degrees C or 530'C. Ten castings were made for each temperature. The images of the castings were analyzed (Leica Qwin) and the castability index determined by the number of the completely cast segments as a percentage of the wax pattern. Data were analyzed by two-way ANOVA and Tukey's multiple comparison test (a = 0.05) using materials and temperatures as discriminating variables.Results. The Ti-6Al-4V alloy (60.86%) presented a better castability index than CP Ti (48.44%) (p < 0.000001). For CP Ti, the temperature of 530 degrees C (23.96%) presented better castability than at other temperatures, 480 degrees C (14.66%) and 430 degrees C (12.54%), with no difference between them (p < 0.001). For Ti-6Al-4V alloy, there was a statistically significant difference among the three temperatures: 530 degrees C (28.36%) > 480 degrees C (19.66%) > 430 degrees C (15.97%) (p < 0.002).Significance. Within the limitations of this study, the increase in the mold temperature of the Rematitan Plus investment resulted in a better castability index for both materials, and Ti-6Al-4V presented a better castability index than CP Ti. (c) 2005 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

An image analysis study of pit formation on Ti-6Al-4V

Metallographic techniques and digital image processing have been used to investigate heat-treated Ti-6Al-4V pitting corrosion, often used as aircraft components. LM and SEM metallography of 'as received', annealed (heating up to 800 degreesC/30 min and cooling furnace) and aged (heating up to 900 degreesC/30 min, quenching in water, heating up to 540 degreesC/240 min and again water-quenched) microstructures reveal pitting sites at primary and secondary alpha/beta interfaces. Microstructural arrangements influence and corrosive environment association on pit morphology could be demonstrated by digital image analysis and results statistical treatment. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Development of Ti-Mo alloys for biomedical applications: Microstructure and electrochemical characterization

Ti-Mo alloys from 4 to 20 Mo wt.% were arc-melted. Their compositions and surfaces were analyzed by EDX, XRF and SEM. The Mo mapping shows a homogeneous distribution for all alloys. The XRD analysis showed that the crystal structure of the alloys is sensitive to the Mo concentration; a mixture of the hexagonal alpha' and orthorhombic alpha '' phases was observed for the Ti-4Mo alloy, and the alpha '' phase is observed almost exclusively when the concentration of Mo added to the Ti reaches 6%. A significant retention of the beta phase is observed for the alloy containing 10% Mo, while at higher Mo concentrations (15% and 20%), retention of phase beta is only verified. Preliminary electrochemical studies have indicated a valve-metal behavior and good corrosion resistance in aerated Ringer solution for all alloys. (c) 2006 Published by Elsevier B.V.

Anelastic relaxation processes due oxygen in Nb-3.1 at.% Ti alloys

In the last 50 years several studies have been made to understand the relaxation mechanisms of the heavy interstitial atoms present in transition metals and their alloys. Internal friction measurements have been carried out in a Nb-Ti alloy containing 3.1 at.% of Ti produced by the Materials Department of Chemical Engineering Faculty of Lorena (Brazil), with several quantities of oxygen in solid solution using a torsion pendulum. These measurements have been performed by a torsion pendulum in the temperature range from 300 to 700 K with an oscillation frequency between 0.5 and 10 Hz. The experimental results show complex internal friction spectra that have been resolved, into a series of Debye peaks corresponding to different interactions. For each relaxation process it was possible to obtain the height and temperature of the peak, the activation energy and the relaxation time of the process. (C) 2003 Elsevier B.V. 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.

Effect of thermal treatments on tensile strength of commercially cast pure titanium and Ti-6Al-4V alloys

Heating titanium structures is assumed to relieve tensions induced by the casting process as well as possibly optimizing some mechanical properties. The aim of this investigation was to evaluate the effect of thermal treatments on tensile strength of commercially pure titanium (CP Ti) and Ti-6Al-4V alloy. Thirty dumbbell rods, with diameters of 3.0 mm at the central segment and lengths of 42 mm, were cast for each metal using the Rematitan System. CP Ti and Ti-6Al-4V specimens were randomly divided into three groups of ten: a control group that received no thermal treatment and two test groups. One (T1) was heated at 750°C for 2 h and the other (T2) was annealed at 955°C for 1 h and aged at 620°C for 2 h. Tensile strength was measured with a universal testing machine (MTS model 810). Tensile strength means and standard deviations were statistically compared using a Kruskal-Wallis test at a α = 0.05 significance level. No statistically significant differences in tensile strength were observed among CP Ti groups. For the Ti-6Al-4V alloy, the control and T1 groups revealed statistically higher tensile strengths when compared to the T2 group, with no significant difference between the control and T1 groups. © 2005 Springer Science + Business Media, Inc.

Influence of thermal and mechanical cycling on the flexural strength of ceramics with titanium or gold alloy frameworks

Objectives: The aim of this study was to evaluate the effect of thermal and mechanical cycling alone or in combination, on the flexural strength of ceramic and metallic frameworks cast in gold alloy or titanium. Methods: Metallic frameworks (25 mm × 3 mm × 0.5 mm) (N = 96) cast in gold alloy or commercial pure titanium (Ti cp) were obtained using acrylic templates. They were airborne particle-abraded with 150 μm aluminum oxide at the central area of the frameworks (8 mm × 3 mm). Bonding agent and opaque were applied on the particle-abraded surfaces and the corresponding ceramic for each metal was fired onto them. The thickness of the ceramic layer was standardized by positioning the frameworks in a metallic template (height: 1 mm). The specimens from each ceramic-metal combination (N = 96, n = 12 per group) were randomly assigned into four experimental fatigue conditions, namely water storage at 37 °C for 24 h (control group), thermal cycling (3000 cycles, between 4 and 55 °C, dwell time: 10 s), mechanical cycling (20,000 cycles under 10 N load, immersion in distilled water at 37 °C) and, thermal and mechanical cycling. A flexural strength test was performed in a universal testing machine (crosshead speed: 1.5 mm/min). Data were statistically analyzed using two-way ANOVA and Tukey's test (α = 0.05). Results: The mean flexural strength values for the ceramic-gold alloy combination (55 ± 7.2 MPa) were significantly higher than those of the ceramic-Ti cp combination (32 ± 6.7 MPa) regardless of the fatigue conditions performed (p < 0.05). Mechanical and thermo-mechanical fatigue decreased the flexural strength results significantly for both ceramic-gold alloy (52 ± 6.6 and 53 ± 5.6 MPa, respectively) and ceramic-Ti cp combinations (29 ± 6.8 and 29 ± 6.8 MPa, respectively) compared to the control group (58 ± 7.8 and 39 ± 5.1 MPa, for gold and Ti cp, respectively) (p < 0.05) (Tukey's test). While ceramic-Ti cp combinations failed adhesively at the metal-opaque interface, gold alloy frameworks exhibited a residue of ceramic material on the surface in all experimental groups. Significance: Mechanical and thermo-mechanical fatigue conditions decreased the flexural strength values for both ceramic-gold alloy and ceramic-Ti cp combinations with the results being significantly lower for the latter in all experimental conditions. © 2007 Academy of Dental Materials.

Crystallographic structure of Ti-6Al-4V, Ti-HP and Ti-CP under high-pressure

The phase stability of a commercial purity (Ti-CP), high purity (Ti-HP) and Ti-6Al-4V alloy were investigated in a diamond anvil cell up to 32 GPa and 298 K using a polychromatic X-ray beam. The Ti-CP and Ti-HP shown the same HCP (c/a∼0.632) to Hexagonal (c/a∼1.63) non reversible martensitic transition at about 9 GPa. The as received Ti-6Al-4V shows a very low relative volume fraction β-Ti / α-Ti. No phase changes were observed in the Ti-6Al-4V alloy in the pressure range of this study. The α phase of the Ti-6Al-4V shows monotonic volume cell pressure dependence. This volume change is reversible and non-hysteretic. The cell of the a phase recovered its original volume when the pressure was released. © 2010 IOP Publishing Ltd.

High-pressure assisted sintering of Ti-20Si-10B and Ti-10Si-5B powders

This work presents the structural characterization of Ti-10Si-5B and Ti-20Si-10B (at-%) alloys produced by high-pressure assisted sintering. Sintering was performed in air at 1100 and 1200°C for 60 s using pressure levels of 5 GPa. Structural evaluation of sintered samples was conducted by means of scanning electron microscopy and energy dispersive spectrometry. Samples were successfully consolidated after sintering, which presented theoretical density values higher than 99%. The microstructures of the sintered Ti-10Si-5B and Ti-20Si-10B alloys revealed the presence of the TiSS, TiB, TiB2, Ti5Si3, Ti5Si4, TiSi, and TiSi2.phases. A small amount of Ti6Si2B was formed after high-pressure assisted sintering of the Ti-20Si-10B alloy (5GPa, 1100°C for 60 s) indicating that equilibrium structures were not achieved during short sintering times. No oxygen and carbon contamination was detected in structures of Ti-Si-B alloys after high-pressure sintering at 1100 and 1200°C without controlled atmosphere. © (2012) Trans Tech Publications, Switzerland.

Analysis on turning Ti-6Al-4V with different cooling methods

The aim of this paper is to optimize the machining of Ti-6Al-4V alloy, by studying the chip formation, roughness and tool wear for different cooling conditions. The results were compared between cooling methods, minimal quantity of fluid (MQF) and flooding, and also without fluid for the tool H13A. The turning of Ti-6Al-4V has shown good results on roughness (0, 8μm) and tool life, which was 11% lower with MQF than with the flooding method. The tool wear causes variation of the shear angle, which promotes strength hardening of the chip. As a result, the machined surface could be damaged. The use of the cutting fluid helps to save the cutting edge and could reduce the strength hardening. Nevertheless, it could also facilitate the formation of built-up edge. The nucleation of alpha lamellar colonies can occur due to a combination of deformation rates and temperature, mainly when the flooding is used, but it's not conclusive. The lamellar colonies were also found with the MQF in some regions, however, this structure did not show hardness variation compared to equiaxial. For all this reasons, the machining parameters might be carefully chosen.