C. J. Boehlert

Biocompatibility and mechanical properties of diamond-like coatings on cobalt-chromium-molybdenum steel and titanium-aluminum-vanadium biomedical alloys

Diamond-like carbon (DLC) films are favored for wear components because of diamond-like hardness, low friction, low wear, and high corrosion resistance (Schultz et al., Mat-wiss u Werkstofftech 2004;35:924-928; Lappalainen et al., J Biomed Mater Res B Appl Biomater 2003;66B:410-413; Tiainen, Diam Relat Mater 2001;10:153-160). Several studies have demonstrated their inertness, nontoxicity, and the biocompatibility, which has led to interest among manufacturers of surgical implants (Allen et al., J Biomed Mater Res B Appl Biomater 2001;58:319-328; Uzumaki et al., Diam Relat Mater 2006;15:982-988; Hauert, Diam Relat Mater 2003;12:583-589; Grill, Diam Relat Mater 2003;12:166-170). In this study, hydrogen-free amorphous, tetrahedrally bonded DLC films (ta-C) were deposited at low temperatures by physical vapor deposition on medical grade Co28Cr6Mo steel and the titanium alloy Ti6Al4V (Scheibe et al., Surf Coat Tech 1996;85:209-214). The mechanical performance of the ta-C was characterized by measuring its surface roughness, contact angle, adhesion, and wear behavior, whereas the biocompatibility was assessed by osteoblast (OB) attachment and cell viability via Live/Dead assay. There was no statistical difference found in the wettability as measured by contact angle measurements for the ta-C coated and the uncoated samples of either Co28Cr6Mo or Ti6Al4V. Rockwell C indentation and dynamic scratch testing on 2-10 μm thick ta-C films on Co28Cr6Mo substrates showed excellent adhesion with HF1 grade and up to 48 N for the critical load L(C2) during scratch testing. The ta-C coating reduced the wear from 3.5 × 10(-5) mm(3)/Nm for an uncoated control sample (uncoated Co28Cr6Mo against uncoated stainless steel) to 1.1 × 10(-7) mm(3)/Nm (coated Co28Cr6Mo against uncoated stainless steel) in reciprocating pin-on-disk testing. The lowest wear factor of 3.9 × 10(-10) mm(3)/Nm was measured using a ta-C coated steel ball running against a ta-C coated and polished Co28Cr6Mo disk. Students t-test found that the ta-C coating had no statistically significant (p < 0.05) effect on OB attachment, when compared with the uncoated control samples. There was no significant difference (p < 0.05) in the Live/Dead assay results in cell death between the ta-C coated Co28Cr6Mo and Ti6Al4V samples and the uncoated controls. Therefore, these ta-C coatings show improved wear and corrosion (Dorner-Reisel et al., Diam Relat Mater 2003;11:823-827; Affato et al., J Biomed Mater Res B Appl Biomater 2000;53:221-226; Dorner-Reisel et al., Surf Coat Tech 2004;177-178:830-837; Kim et al., Diam Relat Mater 2004;14:35-41) performance and excellent in vitro cyto-compatibility, when compared with currently used uncoated Co28Cr6Mo and Ti6Al4V implant materials.

Effect of thermomechanical processing on the creep behaviour of Udimet alloy 188

Udimet alloy 188 was subjected to grain-boundary engineering involving thermomechanical processing in an attempt to improve the creep performance and determine the effects on creep deformation processes. The as-received sheet was cold-rolled to either 10, 25 or 35% reduction per pass followed by a solution treatment at 1191°C for 1 h plus air cooling. This sequence was repeated four times and the resultant microstructure and grain-boundary character distribution were described using electron backscatter diffraction. The fraction of general high-angle grain boundaries tended to increase with increased cold rolling. The 10 and 25% cold-rolled materials exhibited lower creep rates than the 35% cold-rolled material. The measured creep stress exponents and activation energies suggested that dislocation creep with lattice self-diffusion was dominant at 760°C for stresses ranging between 100 and 220 MPa. A transition in the creep exponent below the applied stresses of 100 MPa indicated that a different secondary creep mechanism was rate-controlling at low stresses. A significant amount of grain-boundary cracking was observed both on the surface and subsurface of deformed samples, but surface cracks were greater in number and size than those within the bulk. The cracking behaviour was similar in both vacuum and air environments, indicating that grain-boundary cracking was not caused by environment. To assess the mechanisms of crack nucleation, in situ scanning electron microscopy was performed during elevated-temperature (T ≤ 760°C) tensile-creep deformation. Sequential secondary electron imaging and electron backscatter diffraction orientation mapping were performed in situ to allow the evolution of crack nucleation and linkage to be followed. Cracking occurred preferentially along general high-angle grain boundaries and less than 15% of the cracks were found on low-angle grain boundaries and coincident site lattice boundaries. A fracture initiation parameter analysis was performed to identify the role of slip system interactions at the boundaries and their impact on crack nucleation. The parameter was successful in separating the population of intact and cracked general high-angle boundaries at lower levels of strain, but not after crack coalescence dominated the fracture process. The findings of this work have significant implications regarding grain-boundary engineering of this alloy and potentially for other alloy systems.

Comparison of the deformation behaviour of commercially pure titanium and Ti-5Al-2.5Sn(wt.%) at 296 and 728 K

The tension and tensile-creep deformation behaviours of a fully-α phase commercially pure (CP) Ti and a near-α Ti–5Al–2.5Sn(wt.%) alloy deformed in situ inside a scanning electron microscope were compared. Tensile tests were performed at 296 and 728 K, while tensile-creep tests were performed at 728 K. The yield stress of CP Ti decreased dramatically with increasing temperature. In contrast, temperature had much smaller effect on the yield stress of Ti–5Al–2.5Sn(wt.%). Electron backscattered diffraction was performed both before and after the deformation, and slip trace analysis was used to determine the active slip and twinning systems, as well as the associated global stress state Schmid factors. In tension tests of CP Ti, prismatic slip was the most likely slip system to be activated when the Schmid factor exceeded 0.4. Prismatic slip was observed over the largest Schmid factor range, indicating that the local stress tensor varies significantly from the global stress state of uniaxial tension. The basal slip activity in Ti–5Al–2.5Sn(wt.%) was observed in a larger faction of grains than in CP Ti. Pyramidal ⟨c + a⟩ slip was more prevalent in CP Ti. Although twinning was an active deformation mode in tension tests of the CP Ti, it was rare in Ti–5Al–2.5Sn(wt.%). During creep, dislocation slip was the primary apparent deformation mechanism in CP Ti, while evidence for dislocation slip was much less apparent in Ti–5Al–2.5Sn(wt.%), where grain boundary sliding was dominant. A robust statistical analysis was carried out to assess the significance of the comparative activity of the different slip systems under the variety of experimental conditions examined.

Analysis of slip activity and heterogeneous deformation in tension and tension-creep of Ti-5Al-2.5Sn (wt %) using in-situ SEM experiments

The deformation behavior of a Ti–5Al–2.5Sn (wt %) near-α alloy was investigated during in-situ deformation inside a scanning electron microscope. Tensile experiments were performed at 296 K and 728 K (≈0.4 T m), while tensile-creep experiments were performed at 728 K and 763 K. Active deformation systems were identified using electron backscattered diffraction-based slip trace analysis. Both basal and prismatic slip systems were active during the tensile experiments. Basal slip was observed for grains clustered around high Schmid factor orientations, while prismatic slip exhibited less dependence on the crystallographic orientation. The tension-creep experiments revealed less slip but more development of grain boundary ledges than in the higher strain rate tensile experiments. Some of the grain boundary ledges evolved into grain boundary cracks, and grain boundaries oriented nearly perpendicular to the tensile axis formed ledges earlier in the deformation process. Grain boundaries with high misorientations also tended to form ledges earlier than those with lower misorientations. Most of the grain boundary cracks formed in association with grains displaying hard orientations, where the c-axis was nearly perpendicular to the tensile direction. For the tension-creep experiments, pronounced basal slip was observed in the lower-stress creep regime and the activity of prismatic slip increased with increasing creep stress and temperature.

In situ analysis of the tensile deformation mechanisms in extruded Mg-1Mn-1Nd (wt%)

An extruded Mg–1Mn–1Nd (wt%) (MN11) alloy was tested in tension in an SEM at temperatures of 323 K (50°C), 423 K (150°C), and 523 K (250°C) to analyse the local deformation mechanisms through in situ observations. Electron backscatter diffraction was performed before and after the deformation. It was found that the tensile strength decreased with increasing temperature, and the relative activity of different twinning and slip systems was quantified. At 323 K (50°C), extension twinning, basal, prismatic ⟨a⟩, and pyramidal ⟨c + a⟩ slip were active. Much less extension twinning was observed at 423 K (150°C), while basal slip and prismatic ⟨a⟩ slip were dominant and presented similar activities. At 523 K (250°C), twinning was not observed, and basal slip controlled the deformation.

Examination of the distribution of the tensile deformation systems in tension and tension-creep of Ti-6Al-4V (wt.%) at 296 K and 728 K

The deformation behaviour of an α + β Ti–6Al–4V (wt.%) alloy was investigated during in situ deformation inside a scanning electron microscopy (SEM). Tensile experiments were performed at 296 and 728 K (~0.4Tm), while a tensile-creep experiment was performed at 728 K and 310 MPa (σ/σys = 0.74). The active deformation systems were identified using electron backscattered diffraction-based slip-trace analysis and SEM images of the specimen surface. The distribution of the active deformation systems varied as a function of temperature. Basal slip deformation played a major role in the tensile deformation behaviour, and the relative activity of basal slip increased with increasing temperature. For the 296 K tension deformation, basal slip was less active than prismatic slip, whereas this was reversed at 728 K. Twinning was observed in both the 296 and 728 K tension experiments; however, no more than 4% of the total deformation systems observed was twins. The tension-creep experiment revealed no slip traces, however grain boundary ledge formation was observed, suggesting that grain boundary sliding was an active deformation mechanism. The results of this work were compared with those from previous studies on commercially pure Ti, Ti–5Al–2.5Sn (wt.%) and Ti–8Al–1Mo–1V (wt.%), and the effects of alloying on the deformation behaviour are discussed. The relative amount of basal slip activity increased with increasing Al content.

Out-of-phase thermomechanical fatigue of titanium composite matrices

Abstract A study was undertaken to evaluate the out-of-phase thermomechanical fatigue behavior of three titanium-based alloys: Ti-15Mo-2.6Nb-3Al-0.2Si, Ti-14Al-21Nb, and Ti-13Al-31Nb. The alloys represent compositions from three classes of Ti alloys which have been considered as matrices for titanium-matrix composites. Several tests of each alloy were performed at various maximum stresses, all with a stress ratio of 0.05, a 3 min cycle period, and a temperature cycle of 150 °C to 650 °C. The fatigue lives are compared evaluating S-N behavior and fracture characteristics. In general, the behavior of the Ti-15Mo-2.6Nb-0.2Si alloy was governed by higher toughness compared to the other two alloys, and the Ti-13Al-31Nb alloy demonstrated improved performance over the Ti-14Al-21Nb alloy. A correlation with existing composite data was noted. The correlation is based on calculated micromechanical stresses in the matrix of the composites and applied stresses on the monolithic materials.

Titanium Alloys for Biomedical Applications

The low Young’s modulus of β-type titanium alloys makes them advantageous for use in medical implant devices, as they are effective in both preventing bone resorption and promoting good bone remodeling. The development of low Young’s modulus β-type titanium alloys for biomedical applications is described herein, along with a discussion of suitable methods for even greater modulus reductions. Since there is often occasion to remove implant devices, titanium alloys suitable for removable implants are also described. It has recently been noted that although patients require low Young’s modulus titanium alloys, a high modulus is needed by surgeons. Consequently, β-type titanium alloys with a self-tunable Young’s modulus are also explored. An evaluation of the effectiveness of low Young’s modulus β-type titanium alloys in preventing stress shielding is provided, which is based on the results of animal testing. Means of enhancing the mechanical biocompatibilities of β-type titanium alloys for biomedical applications are also described along with the suitability of those β-type titanium alloys which exhibit super-elastic and shape-memory behavior. Finally, the unique behavior of some β-type titanium alloys for biomedical applications is discussed.

Abnormal Deformation Behavior of Oxygen-Modified β-Type Ti-29Nb-13Ta-4.6Zr Alloys for Biomedical Applications

Abstract Oxygen was added to the biomedical β-type Ti-29Nb-13Ta-4.6Zr alloy (TNTZ, mass pct) in order to improve its strength, while keeping its Young’s modulus low. Conventionally, with an increase in the oxygen content, an alloy’s tensile strength increases, while its tensile elongation-to-failure decreases. However, an abnormal deformation behavior has been reported in the case of oxygen-modified TNTZ alloys in that their strength increases monotonically while their elongation-to-failure initially decreases and then increases with the increase in the oxygen content. In this study, this abnormal tensile deformation behavior of oxygen-modified TNTZ alloys was investigated systematically. A series of TNTZ-(0.1, 0.3, and 0.7 mass pct)O alloy samples was prepared, treated thermomechanically, and finally solution treated; these samples are denoted as 0.1ST, 0.3ST, and 0.7ST, respectively. The main tensile deformation mechanisms in 0.1ST are a deformation-induced α″-martensitic transformation and {332}〈113〉 mechanical twinning. The large elongation-to-failure of 0.1ST is attributable to multiple deformation mechanisms, including the deformation-induced martensitic transformation and mechanical twinning as well as dislocation glide. In both 0.3ST and 0.7ST, dislocation glide is the predominant deformation mode. 0.7ST shows more homogeneous and extensive dislocation glide along with multiple slip systems and a higher frequency of cross slip. As a result, it exhibits a higher work-hardening rate and greater resistance to local stress concentration, both of which contribute to its elongation-to-failure being greater than that of 0.3ST.

In-Situ Study of the Tensile Deformation and Fracture Modes in Peak-Aged Cast Mg-11Y-5Gd-2Zn-0.5Zr (Weight Percent)

Tensile deformation and fracture modes in peak-aged cast Mg-11Y-5Gd-2Zn-0.5Zr (wt pct) (WGZ1152) samples at temperatures between 298 K [25 °C, room temperature (RT)] and 623 K (350 °C) (0.33 to 0.69Tm) were studied in situ inside a scanning electron microscope (SEM) using electron backscatter diffraction (EBSD) and slip trace analysis. The ultimate tensile strength (UTS) (265 MPa) and yield strength (YS) (193 MPa) at 523 K (250 °C) were 91 and 80 pct of those at RT, respectively. The observed dominant slip mode transitioned from basal 〈a〉 slip (100 pct) to basal 〈a〉 slip (81 pct) combined with prismatic 〈a〉 slip (12 pct) from RT to 473 K (200 °C). As the temperature increased to 623 K (350 °C), basal 〈a〉 slip (67 pct) and pyramidal 〈c+a〉 slip (25 pct) became the dominant slip modes. The estimated critical resolved shear stress (CRSS) ratio of pyramidal 〈c+a〉 slip/basal 〈a〉 slip (7.3) was lower than that of prismatic 〈a〉 slip/basal 〈a〉 slip (12.7) at temperatures above 573 K (300 °C). Prismatic 〈a〉 slip and pyramidal 〈c+a〉 slip were more active at higher strains for moderate temperatures [473 K to 523 K (200 °C to 250 °C)] and at high temperatures [573 K to 623 K (300 °C to 350 °C)], respectively. A transition in the dominant fracture mode occurred from transgranular cracking (40 pct) combined with intergranular cracking (60 pct) to intergranular cracking as temperatures increased from RT to 623 K (350 °C). The intergranular crack nucleation sites tended to be located at grain boundaries and the interface between the Mg matrix and the large intermetallic grain boundary X phase. Slip bands were associated with transgranular crack nucleation.