Fatigue and wear evaluation of Ti-Al-Nb alloys for biomedical applications

In this work the fatigue and wear behavior of Ti–15Al–33Nb(at.%) and Ti–21Al–29Nb(at.%) was evaluated and compared to that for other titanium-based biomedical implant alloys, in particular Ti–6Al–4V(wt.%). Fatigue stress versus life curves were obtained for tests performed at room temperature in air at a stress ratio of R = 0.1 for maximum stresses between 75%–90% of the ultimate tensile strength. The results indicated that the fatigue strength and lives of the as-processed alloys are comparable to that for Ti–6Al–4V(wt.%). Heat treatment significantly increased the orthorhombic-phase volume fractions in the alloys and resulted in reduced fatigue strength. The wear resistance for the alloys was significantly greater than that for Ti–6Al–4V(wt.%). Based on the current results, it is proposed that titanium–aluminum–niobium alloys will be of considerable future interest for biomedical applications.     

Surface characterization and biocompatibility of titanium alloys implanted with nitrogen by Hardion+ technology

In this study, the new Hardion+ micro-implanter technology was used to modify surface properties of biomedical pure titanium (CP-Ti) and Ti?C6Al?C4V ELI alloy by implantation of nitrogen ions. This process is based on the use of an electron cyclotron resonance ion source to produce a multienergetic ion beam from multicharged ions. After implantation, surface analysis methods revealed the formation of titanium nitride (TiN) on the substrate surfaces. An increase in superficial hardness and a significant reduction of friction coefficient were observed for both materials when compared to non-implanted samples. Better corrosion resistance and a significant decrease in ion release rates were observed for N-implanted biomaterials due to the formation of the protective TiN layer on their surfaces. In vitro tests performed on human fetal osteoblasts indicated that the cytocompatibility of N-implanted CP-Ti and Ti?C6Al?C4V alloy was enhanced in comparison to that of the corresponding non treated samples. Consequently, Hardion+ implantation technique can provide titanium alloys with better qualities in terms of corrosion resistance, cell proliferation, adhesion and viability.     

Mechanical properties and microstructures of new Ti–Fe–Ta and Ti–Fe–Ta–Zr system alloys

β-type titanium alloys consisting of non-toxic elements, Ti–8Fe–8Ta, Ti–8Fe–8Ta–4Zr, and Ti–10Fe–10Ta–4Zr, were newly designed and developed for biomedical applications. Changes in the mechanical properties of the designed alloys with various heat treatments were discussed on the basis of the resultant microstructures. In addition, the corrosion resistance of the designed alloys was evaluated by polarization testing in Hank's solution. Conventional biomedical titanium (cp-Ti) and the titanium alloy Ti–6Al–4V ELI were also polarized for comparison.The structural phase of the designed alloys, after cold rolling and solution treatment, was only the β phase. Ultimate tensile strength and elongation to fracture of Ti–8Fe–8Ta, Ti–8Fe–8Ta–4Zr, and Ti–10Fe–10Ta–4Zr after solution treatment were 1066 MPa and 10%, 1051 MPa and 10%, and 1092 MPa and 6%, respectively. Ti–8Fe–8Ta and Ti–8Fe–8Ta–4Zr have higher strength than those of conventional biomedical titanium alloys such as Ti–6Al–4V ELI, Ti–6Al–7Nb, and Ti–13Nb–13Zr. In particular, the elongations at failure of Ti–8Fe–8Ta and Ti–8Fe–8Ta–4Zr were equal to those of Ti–6Al–4V ELI and Ti–6Al–7Nb. The designed alloys and conventional biomedical titanium alloys were spontaneously passivated in Hank's solution. The current density of cp-Ti and Ti–6Al–4V ELI was increased at a potential above 2.5 V. On the other hand, the current density of the designed alloys abruptly increased at a potential above 3.5 V. The designed alloys have the advantage over cp-Ti and Ti–6Al–4V ELI in their high resistance to pitting corrosion in biological environments.Therefore, new β-type titanium alloys designed in this study, Ti–8Fe–8Ta and Ti–8Fe–8Ta–4Zr, are expected to have good properties as biomaterials.     

钛合金表面加弧辉光离子渗镍铬及其性能研究

采用加弧辉光离子渗金属新技术处理钛合金Ti5Al2.5Sn表面,研究了渗层的相组成特点,成分分布情况,评价了改性层的磨擦摩损性能,及与钛合金基体间的接触腐蚀相容性等。结果表明加弧辉光离子渗技术可以快速地在钛合金表面获得NiCr镀渗复合层。渗层由Ni3Ti等金属间化合物组成,其硬度、耐磨性能均高于离子注氮层,具有较高的抗含Cl^-1水溶液腐蚀性能,在含Cl^-1腐蚀环境中与钛合金基体接触相容。     

Evaluation of cast Ti–Fe–O–N alloys for dental applications

Good mechanical properties, biocompatibility and corrosion resistance make titanium an excellent material for biomedical applications. However, when better mechanical properties than those offered by commercially pure titanium (CPTi) are needed, Ti–6Al–4V is sometimes a good alternative. Some new titanium alloys, developed as industrial structural materials, aim at an intermediate range of strength between that of CP Ti and Ti–6Al–4V. Two of these alloys are Super-TIX800™ (Ti–1% Fe–0.35% O–0.01% N) and Super-TIX800N™ (Ti–1% Fe–0.3% O–0.04% N) (both produced by Nippon Steel Corp., Japan). Besides being stronger than CP Ti, the cost of manufacturing these alloys is reportedly lower than for Ti–6Al–4V since they do not contain any expensive elements. In addition, they are not composed of elements such as aluminum or vanadium, which have caused biocompatibility concerns in medical and dental appliances. To evaluate these alloys as candidates for dental use, it is helpful to compare them to CP Ti (ASTM Grade 2) and Ti–6Al–4V (ASTM Grade 5), which have already been employed in dentistry. We evaluated the tensile properties, mold filling capacity, corrosion characteristics and grindability of these industrial alloys prepared by investment casting. Compared to the strengths of cast CPTi, the yield strength and tensile strength of these cast alloys were more than 20% and approximately 30% higher, respectively. On the other hand, both of these properties were 30% lower than for Ti–6Al–4V. Better grindability and wear resistance were additional benefits of these new alloys for dental applications.     

Effect of Vacuum Heat Treatment on the Microstructure and Tribological Property of Ti–6Al–4V Alloy with Cu Coating

The effect of vacuum heat treatment on the interface microstructure and tribological property of Cu-coated Ti – 6Al – 4V alloy is investigated herein. After the vacuum heat treatment process, a diffusion layer is formed at the interface between the Cu coating and the Ti – 6Al – 4V substrate. The formed intermetallic compounds at the interface between the Ti – 6Al – 4V substrate and Cu coating are CuTi₂, CuTi, Cu₄Ti₃, and β-Cu₄Ti. The activation energy of intermetallic compound growth in the diffusion zone of Cu-coated Ti – 6Al – 4V is 126.0 kJ mol⁻¹, and the pre-exponential factor is 0.1 m² s⁻¹. The tribological properties of the Cu-coated Ti – 6Al – 4V alloy are best when subjected to diffusion treatment at 700 °C for 300 min, with weight loss reduced by 58.2% compared to the Ti – 6Al – 4V alloy. The wear resistance of the Ti – 6Al – 4V alloy can be enhanced by Cu coating and vacuum diffusion heat treatment, and the formation of the Cu – Ti intermetallic compound contributes to this improvement. These findings offer new insights for further advancements in the tribological properties of titanium alloys.     

Ti6Al4V合金双辉渗钼扩散系数的数值分析

以Ti6A14V合金双辉等离子渗钼的扩散行为为研究对象,针对具有沉积层和扩散层的典型钼合金化改性层的钼元素含量分布形态,采用数值分析方法计算了钼元素的扩散系数。结果表明:通过这种数值计算方法能较好地揭示Ti6A14V合金等离子渗钼的扩散行为,高钼浓度区域的钼扩散系数较小,而低钼浓度区域的钼扩散系数较大;不同沉积层的处理方法对钼扩散系数的计算结果影响显著。     

Evaluation of the effects of plasma nitriding temperature and time on the characterisation of Ti 6Al 4V alloy

The effects of plasma nitriding (PN) temperature and time on the structural and tribological characterisation of Ti 6Al 4V alloy were investigated. PN processes under gas mixture of N₂/H₂ = 4 were performed at temperatures of 700, 750, 800 and 850 °C for duration of 2, 5 and 10 h. Cross section and surface characterisation were evaluated by means of SEM, AFM, XRD and microhardness test techniques. Dry wear tests were performed using a pin on disc machine. Mass loss and coefficient of friction were measured during the wear tests. Three distinguished structures including of a compound layer (constituted of δ-TiN and ɛ-Ti₂N), an aluminium-rich region and a diffusion zone (interstitial solid solution of nitrogen in titanium) were detected at the surface of plasma nitrided Ti 6Al 4V alloy. These structures increased surface hardness of Ti 6Al 4V alloy significantly and gradually distributed the hardness from the surface to the substrate. The "surface hardness", "surface roughness", "wear resistance" and "coefficient of friction" of the alloy were increased due to plasma nitriding process. Moreover, rising both process temperature and time led to increasing of "layers thicknesses", "surface hardness", "surface roughness", "dynamic load-ability" and "wear resistance" of Ti 6Al 4V alloy.     

Three-dimensional mixed-mode fatigue crack growth in a functionally graded titanium alloy

The implementation of unitized structure in the aerospace industry has resulted in complex geometries and load paths. Hence, structural failure due to three-dimensional mixed-mode fatigue crack growth is a mounting concern. In addition, the development of functionally graded materials has further complicated structural integrity issues by intentionally introducing material variability to create desirable mechanical behavior. Ti-6Al-4V β-STOA (solution treated over-aged) titanium is a functionally graded metallic alloy that has been tailored for superior fatigue crack growth and fracture response compared with traditional titanium alloys. Specifically, the near-surface material of Ti β-STOA is resistant to fatigue crack incubation and the interior is more resistant to fatigue crack growth and fracture. Therefore, Ti β-STOA is well suited for applications where surface cracking is a known failure mode. Advances in experimental testing have shown that complex loading conditions and multi-faceted materials can be tested reliably. In this paper, the authors will experimentally generate three-dimensional mixed-mode surface crack data in functionally graded Ti-6Al-4V β-STOA and comment on the effect of the material tailoring.     

Effect of shotpeening on sliding wear and tensile behavior of titanium implant alloys

Titanium has good biocompatibility and so its alloys are used as implant materials, but they suffer from having poor wear resistance. This research aims to improve the wear resistance and the tensile strength of titanium alloys potentially for implant applications. Titanium alloys Ti–6Al–4V and Ti–6Al–7Nb were subjected to shotpeening process to study the wear and tensile behavior. An improvement in the wear resistance has been achieved due to surface hardening of these alloys by the process of shotpeening. Surface microhardness of shotpeened Ti–6Al–4V and Ti–6Al–7Nb alloys has increased by 113 and 58 HV_(0.5), respectively. After shotpeening, ultimate tensile strength of Ti–6Al–4V increased from 1000 MPa to 1150 MPa, higher than improvement obtained for heat treated titanium specimens. The results confirm that shotpeening pre-treatment improved tensile and sliding wear behavior of Ti–6Al–4V and Ti–6Al–7Nb alloys. In addition, shotpeening increased surface roughness.     

Corrosion behavior of biomedical Ti–24Nb–4Zr–8Sn alloy in different simulated body solutions

Corrosion behavior of a multifunctional biomedical titanium alloy Ti–24Nb–4Zr–8Sn (wt.%) in 0.9% NaCl, Hank's solution and artificial saliva at 37 °C was investigated using open circuit potential, impedance spectroscopy and potentiodynamic polarization techniques, and some results were compared with pure titanium and Ti–6Al–4V alloy. The results showed that the alloy exhibited good corrosion resistance due to the formation of a protective passive film consisting mainly of TiO₂ and Nb₂O₅, and a little of ZrO₂ and SnO₂. Ca ions were detected in the passive film as the alloy immersed in Hank′s and artificial saliva solutions and they have negative effect on corrosion resistance. The EIS results indicated that either a duplex film with an inner barrier layer and an outer porous layer or a single passive layer was formed on the surface, and they all transformed into stable bilayer structure as the immersion time increased up to 24 h. The polarization curves demonstrated that the alloy had a wider passive region than pure titanium and Ti–6Al–4V alloy and its corrosion current density (less than 0.1 μA/cm²) is comparable to that of pure titanium.     

Ti–6Al–4V–0.5B—A Modified Alloy for Implants Produced by Metal Injection Molding

Permanent implants have to fulfill a great variety of requirements related to both material and geometry. In addition, manufacturing costs play a role, which is getting steadily more and more important. Metal Injection Molding (MIM) of titanium alloy powders may contribute to the development of implants with higher functionality without increasing the price. High degree of freedom with regard to geometry, high material efficiency, and the possibility to create even porous structures are main benefits from applying this technique. Today, even long‐term implants made from Ti–6Al–4V by MIM are commercially available. However, in order to improve fatigue behavior it is beneficial to perform a minor variation of Ti–6Al–4V by adding a low amount of boron. In this paper the mechanical, biological, and corrosion properties of specimens manufactured from Ti–6Al–4V–0.5B alloy by MIM are presented. In order to exclude unknown reactions in the body environment due to the boron content, corrosion, and biological tests are performed. Tensile and fatigue tests characterize the mechanical properties. Potentiodynamic polarization and electrochemical impedance spectroscopy are done in comparison to wrought and to MIM processed Ti–6Al–4V material. For cell experiments cancellous bone cells are cultured to perform adhesion, proliferation, and viability experiments. The results presented here show that the alloy Ti–6Al–4V–0.5B satisfies all basic needs of a material for highly loaded permanent implants manufactured by MIM.     

钛合金表面磁控溅射离子渗镀铜的烧蚀特性研究

针对一定条件下钛合金的易燃以及在双层辉光离子渗铜中铜源极易熔的问题,采用了磁控溅射的技术,在Ti6Al4V的表面进行铜元素的渗镀,形成的Ti-Cu阻燃合金层以提高其阻燃性能.研究溅射功率、溅射时间、工作气压等工艺参数对铜渗镀层厚度的影响后,发现0.6 Pa的工作气压、180 W的溅射功率、3 h的溅射时间为优化工艺参数.XRD结构分析表明,Ti6Al4V样品表面形成了含CuTi2相的合金层;激光烧蚀实验表明,钛合金渗铜层的阻燃性能提高了2倍以上,但表面纯铜薄膜层对阻燃性能没有帮助.     

电火花表面强化与喷丸复合处理对Ti811合金高温微动疲劳性能的影响

研究了Ti811钛合金表面电火花强化层的界面成分分布、耐磨和微动疲劳性能.研究结果表明:以0Cr18Ni9合金为电极材料在Ti811钛合金表面进行电火花处理可以形成合金层,显著提高了钛合金表面硬度和耐磨性能.但由于合金层硬度高,韧性较低,在微动疲劳(FF)过程中易萌生裂纹并快速扩展进入基体,致使高温下钛合金FF抗力降低.对电火花强化层进行喷丸强化(SP)后处理能够使钛合金FF抗力恢复到裸件的水平.     

High‐cycle fatigue properties of beta Ti alloy 55Ti–30Nb–10Ta–5Zr,gum metal

This paper describes the fatigue properties of the beta titanium alloy 55Ti–30Nb–10Ta–5Zr, generally referred to as ‘Gum Metal’. Rotating bending fatigue tests have been performed in laboratory air and in a 3% NaCl aqueous solution. The results obtained were compared with those of a conventional beta titanium alloy, Ti–22V–4Al. In tensile tests, 55Ti–30Nb–10Ta–5Zr indicated elasticity and microplasticity in the elastic region. Thus, the elastic modulus slightly decreased with an increasing strain, and the work hardening was minimal during plastic deformation. The mechanical properties of both of the alloys were comparable. The fatigue strength of 55Ti–30Nb–10Ta–5Zr in laboratory air was higher than that of Ti–22V–4Al, which could be attributed to the higher fatigue crack initiation resistance of 55Ti–30Nb–10Ta–5Zr than Ti–22V–4Al, while the resistance to small fatigue crack growth was similar. The fatigue strength of 55Ti–30Nb–10Ta–5Zr in laboratory air and in the 3% NaCl aqueous solution was analogous. In addition, corrosion pits were not observed in the run‐out specimen in the 3% NaCl aqueous solution, indicating a high resistance of 55Ti–30Nb–10Ta–5Zr against corrosion fatigue.     

Verhalten laserschockverfestigter und festgewalzter Randschichten der Ti‐Legierung Ti‐6Al‐4V bei schwingender Beanspruchung unter erhöhten Temperaturen

Residual stress stability and near‐surface microstructures in high temperature fatigued mechanically surface treated Ti‐6Al‐4V It is well known that mechanical surface treatments, such as deep rolling, shot peening and laser shock peening, can significantly improve the fatigue behavior of highly‐stressed metallic components. Deep rolling is particularly attractive since it is possible to generate, near the surface, deep compressive residual stresses and work hardened layers while retaining a relatively smooth surface finish. In the present investigation, the effect of deep rolling on the low‐cycle and high‐cycle fatigue behavior of a Ti‐6Al‐4V alloy is examined, with particular emphasis on the thermal and mechanical stability of the residual stress states and the near‐surface microstructures. Preliminary results on laser shock peened Ti‐6Al‐4V are also presented for comparison. Particular emphasis is devoted to the question of whether such surface treatments are effective for improving the fatigue properties at elevated temperatures up to ～450 °C, i.e., at an homologous temperature of ～0.4 T/T_m (where T_m is the melting temperature). Based on cyclic deformation and stress/life (S/N) fatigue behavior, together with the X‐ray diffraction and in situ transmission electron microscopy observations of the microstructure, it was found that deep rolling can be quite effective in retarding the initiation and initial propagation of fatigue cracks in Ti‐6Al‐4V at such higher temperatures, despite the almost complete relaxation of the near‐surface residual stresses. In the absence of such stresses, it is shown that the near‐surface microstructures, which in Ti‐6Al‐4V consist of a layer of work hardened nanoscale grains, play a critical role in the enhancement of fatigue life by mechanical surface treatment.     

Local strain accumulation in fatigue crack propagation process of Ti‐6Al‐4V alloy

Fatigue crack growth behaviours of the titanium alloy Ti‐6Al‐4V, with two different microstructures, at different maximum stresses were identified by digital image correlation technique. Full‐field strains were monitored around fatigue cracks after consecutive cycles in fatigue crack growth experiments. Results indicated that the Ti‐6Al‐4V alloy with a bi‐modal microstructure had a better fatigue resistance than that with a primary‐α microstructure. Typical behaviours of small cracks and the evolution of multi‐scale fatigue cracks were clarified. The strain accumulations around the micro‐notch and fatigue crack increased with increasing number of load cycles. On the basis of von Mises strain mapping, it was found that crack growth rate could be characterized by crack‐tip plastic zone size.     

Osteoblast cell behavior on the new beta-type Ti–25Ta–25Nb alloy

Among metallic materials used as bone substitutes, β titanium alloys gain an increasing importance because of their low modulus, high corrosion resistance and good biocompatibility. In this work, an investigation of the in vitro cytocompatibility of a recently new developed β-type Ti–25Ta–25Nb alloy was carried out by evaluating the behavior of human osteoblasts. The metallic Ti–6Al–4V biomaterial, which is one of representative α + β type titanium alloys for biomedical applications, and Tissue Culture Polystyrene (TCPS), were also investigated as reference Ti-based material and control substrate, respectively. Both metallic surfaces were analyzed by X-ray diffraction, atomic force microscopy and X-ray photoelectron spectroscopy. The cellular response was quantified by assessments of viability, cell attachment and spreading, cell morphology, production and extracellular organization of fibronectin and cell proliferation. Polished surfaces from both materials having an equiaxed grain microstructure and nanometre scale surface roughness elicited an essentially identical osteoblast response in terms of all analyzed cellular parameters. Thus, on both surfaces the cells displayed high survival rates, good cell adhesion and spreading, a dense and randomly dispersed fibronectin matrix and increasing cell proliferation rates over the incubation time. Furhermore, the enhanced biological performance of Ti–25Ta–25Nb was highly supported by the results obtained in comparison with TCPS. These findings, together with previously shown superelastic behavior, low Young's modulus and high corrosion resistance, recommend Ti–25Ta–25Nb as good candidate for applications in bone implantology.     

激光冲击处理对Ti6Al4V力学性能的影响

通过对钛合金Ti6Al4V的激光冲击处理,研究了激光冲击处理工艺对钛合金Ti6Al4V力学性能的影响.实验表明:激光冲击处理能有效提升Ti6Al4V的力学性能,在激光功率密度由1.15GW/cm2增加到2.31GW/cm2过程中,其冲击波峰值压力线性增加,表面最大残余压应力也相应增大,最高达-264MPa,表面硬化层的显微硬度高达510Hv,硬化层深度约为0.25mm,经过激光冲击处理后硬度相对于原始钛板提高了64%,随着激光能量的增加,冲击区域的抗拉强度极大增强,塑性降低.     

Ti6Al4V钛合金表面Ta2O5/Ta2O5-Ti/Ti多涂层的制备与性能研究

采用磁控溅射技术在Ti6Al4V钛合金表面制备了Ta_2O_5/Ta_2O_5-Ti/Ti多层涂层;利用扫描电子显微镜(SEM)、X射线衍射仪(XRD)和X射线光电子能谱仪 (XPS),分析了涂层的微观结构、物性组成和化学价态;通过划痕仪、纳米压痕仪、摩擦磨损试验机和电化学工作站,检测了涂层的结合强度、力学性能、摩擦系数和耐腐蚀性。研究结果表明,Ta_2O_5/Ta_2O_5-Ti/Ti多层涂层表面由峰型颗粒组成,粒径大小均匀,涂层结构致密。与Ti6Al4V相比,Ta_2O_5/Ta_2O_5-Ti/Ti多层涂层试样具有较小的摩擦系数,较高的腐蚀电位和较小的腐蚀电流密度,表现出良好的耐磨和耐腐蚀性能,能对Ti6Al4V合金植入材料起到较好的保护作用。