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In bcc metastable ß titanium alloys, and particularly in superelastic alloys, a unique {332}⟨113⟩ twinning system occurs during plastic deformation. However, in situ synchrotron x-ray diffraction during a tensile test shows that the ß phase totally transforms into α^{''} martensite under stress in a Ti-27Nb (at. %) alloy. {332}⟨113⟩_{ß} twins are thus not formed directly in the ß phase but are the result of the reversion of {130}⟨310⟩_{α^{''}} parent twins occurring in martensite under stress. The formation of an interfacial twin boundary ω phase is also observed to accommodate strains induced during the phase reversion.

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In this study, the "Gum Metal" titanium-based alloy (Ti-23Nb-0.7Ta-2Zr-1.2O) was synthesized by melting and then characterized in order to evaluate its potential for biomedical applications. Thus, the mechanical properties, the corrosion resistance in simulated body fluid and the in vitro cell response were investigated. It was shown that this alloy presents a very high strength, a low Young's modulus and a high recoverable strain by comparison with the titanium alloys currently used in medicine. On the other hand, all electrochemical and corrosion parameters exhibited more favorable values showing a nobler behavior and negligible toxicity in comparison with the commercially pure Ti taken as reference. Furthermore, the biocompatibility tests showed that this alloy induced an excellent response of MC3T3-E1 pre-osteoblasts in terms of attachment, spreading, viability, proliferation and differentiation. Consequently, the "Gum Metal" titanium-based alloy processes useful characteristics for the manufacturing of highly biocompatible medical devices.

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In this study, a superelastic Ni-free Ti-based biomedical alloy was treated in surface by the implantation of nitrogen ions for the first time. The N-implanted surface was characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and secondary ion mass spectroscopy, and the superficial mechanical properties were evaluated by nano-indentation and by ball-on-disk tribological tests. To investigate the biocompatibility, the corrosion resistance of the N-implanted Ti alloy was evaluated in simulated body fluids (SBF) complemented by in-vitro cytocompatibility tests on human fetal osteoblasts. After implantation, surface analysis methods revealed the formation of a titanium-based nitride on the substrate surface. Consequently, an increase in superficial hardness and a significant reduction of friction coefficient were observed compared to the non-implanted sample. Also, a better corrosion resistance and a significant decrease in ion release rates have been obtained. Cell culture experiments indicated that the cytocompatibility of the N-implanted Ti alloy was superior to that of the corresponding non-treated sample. Thus, this new functional N-implanted titanium-based superelastic alloy presents the optimized properties that are required for various medical devices: superelasticity, high superficial mechanical properties, high corrosion resistance and excellent cytocompatibility.

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Thermomechanical treatments have been proved to be an efficient way to improve superelastic properties of metastable ß type titanium alloys through several studies. In this paper, this treatment routes, already performed on superelastic alloys, are applied to the Ti-24Nb alloy (at%) consisting of a pure martensite α'' microstructure. By short-time annealing treatments performed on the heavily deformed material, an interesting combination of a large recoverable strain of about 2.5%, a low elastic modulus (35 GPa) and a high strength (900 MPa) was achieved. These properties are shown to be due to a complex microstructure consisting of the precipitation of nanoscale (α+ω) phases in ultra-fine ß grains. This microstructure allows a superelastic behavior through stress-induced α'' martensitic transformation. In this study, the microstructures were characterized by X-ray diffraction and transmission electron microscopy and the evolution of the elastic modulus and the strain recovery as a function of the applied strain was investigated through loading-unloading tensile tests.

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In this study, the new Hardion+ micro-implanter technology was used to modify surface properties of biomedical pure titanium (CP-Ti) and Ti-6Al-4V 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-6Al-4V 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.

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In this study, the microstructure and the mechanical properties of two new biocompatible superelastic alloys, Ti-24Nb-0.5O and Ti-24Nb-0.5N (at.%), were investigated. Special attention was focused on the role of O and N addition on α(″) formation, supereleastic recovery and mechanical strength by comparison with the Ti-24Nb and Ti-26Nb (at.%) alloy compositions taken as references. Microstructures were characterized by optical microscopy, X-ray diffraction and transmission electron microscopy before and after deformation. The mechanical properties and the superelastic behavior were evaluated by conventional and cyclic tensile tests. High tensile strength, low Young's modulus, rather high superelastic recovery and excellent ductility were observed for both superelastic Ti-24Nb-0.5O and Ti-24Nb-0.5N alloys. Deformation twinning was shown to accommodate the plastic deformation in these alloys and only the {332}<113> twinning system was observed to be activated by electron backscattered diffraction analyses.

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A flash-thermal treatment technique has been developed very recently to improve both the critical stress to induce the martensitic transformation (MT) and the recoverable deformation of the metastable ß type titanium alloys. In this paper, this strategy is applied to both Ti-26Nb and Ti-20Nb-6Zr (at.%) alloys. Since both alloys have identical martensite start (Ms) temperature, it makes possible to investigate the effect of Zr on mechanical properties after the flash-thermal treatment. It is clearly shown that a flash treatment of 360 s at 873 K on heavily cold-rolled samples results in good balance between the tensile strength, the ductility and the recoverable strains. Such contribution is more significant in the ternary alloy in which balanced properties combining high martensitic critical stress over 400 MPa and the large fully recoverable strains up to 3.0% can be achieved. These improvements are due to the flash treatment effects, resulting in ultra-fine ß grains with sizes 1-2 µm with nano-sized α and ω phases precipitation in the ß matrix.

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In this study, a new Ti-25Ta-25Nb (mass%) beta alloy was synthesised by cold crucible semi-levitation melting. This technique made it possible to obtain homogeneous ingots although the elements used have very different melting points. After melting, a thermo-mechanical treatment was applied in order to obtain a perfectly recrystallised beta microstructure. For this alloy composition, the tensile tests showed a very low Young's modulus associated with an important super-elastic behaviour, which contributes to decrease the elastic modulus under stress and to increase the recoverable strain. On the other hand, the corrosion tests, which were carried out in a neutral Ringer solution, indicated a corrosion resistance higher than that of the commercially pure CP Ti alloy. These results show that this new alloy possesses all the characteristics necessary for its long-term use in medical implants.

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Titanium alloys dedicated to biomedical applications may display both clinical and mechanical biocompatibility. Based on nontoxic elements such as Ti, Zr, Nb, Ta, they should combine high mechanical resistance with a low elastic modulus close to the bone elasticity (E=20 GPa) to significantly improve bone remodelling and osseointegration processes. These elastic properties can be reached using both lowering of the intrinsic modulus by specific chemical alloying and superelasticity effects associated with a stress-induced phase transformation from the BCC metastable beta phase to the orthorhombic alpha(″) martensite. It is shown that the stability of the beta phase can be triggered using a chemical formulation strategy based on the electronic design method initially developed by Morinaga. This method is based on the calculation of two electronic parameters respectively called the bond order (B(o)) and the d orbital level (M(d)) for each alloy. By this method, two titanium alloys with various tantalum contents, Ti-29Nb-11Ta-5Zr and Ti-29Nb-6Ta-5Zr (wt%) were prepared. In this paper, the effect of the tantalum content on the elastic modulus/yield strength balance has been investigated and discussed regarding the deformation modes. The martensitic transformation beta-->alpha(″) has been observed on Ti-29Nb-6Ta-5Zr in contrast to Ti-29Nb-11Ta-5Zr highlighting the chemical influence of the Ta element on the initial beta phase stability. A formulation strategy is discussed regarding the as-mentioned electronic parameters. Respective influence of cold rolling and flash thermal treatments (in the isothermal omega phase precipitation domain) on the tensile properties has been investigated.

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We have synthesized titanium-based alloys containing molybdenum and tantalum elements by powder metallurgy. The microstructure, the residual porosity and the mechanical properties of the sintered Ti-Mo and Ti-Ta-Mo alloys were investigated by using optical and electronic microscopy, X-ray diffraction, microhardness and compression tests. The cytocompatibility of the different alloys was evaluated by the assessment of bone cell density, migration and adhesion after 14 days incubation. All the alloys present a high ductility and an excellent cytocompatibility, which make these materials useful for medical implants.

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Ti-based biocompatible alloys are especially used for replacing failed hard tissue. Some of the most actively investigated materials for medical implants are the beta-Ti alloys, as they have a low elastic modulus (to inhibit bone resorption). They are alloyed with elements such as Nb, Ta, Zr, Mo, and Fe. We have prepared a new beta-Ti alloy that combines Ti with the non-toxic elements Ta and Mo using a vacuum arc-melting furnace and then annealed at 950 degrees C for one hour. The alloy was finally quenched in water at room temperature. The Ti-12Mo-5Ta alloy was characterised by X-ray diffraction, optical microscopy, SEM and EDS and found to have a body-centred-cubic structure (beta-type). It had a lower Young's modulus (about 74 GPa) than the classical alpha/beta Ti-6Al-4V alloy (120 GPa), while its Vickers hardness remained very high (about 303 HV). This makes it a good compromise for a use as a bone substitute. The cytocompatibility of samples of Ti-12Mo-5Ta and Ti-6Al-4V titanium alloys with various surface roughnesses was assessed in vitro using organotypic cultures of bone tissue and quantitative analyses of cell migration, proliferation and adhesion. Mechanically polished surfaces were prepared to produce unorientated residual polished grooves and cells grew to a particularly high density on the smoother Ti-12Mo-5Ta surface tested.

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Parallel to the biofunctionalisation of existing materials, innovation in biomaterials engineering has led to the specific design of titanium alloys for medical applications. Studies of the biological behaviour of metallic elements have shown that the composition and structure of the material should be carefully tailored to minimise adverse body reactions and to enhance implant longevity, respectively. Consequently, interest has focused on a new family of titanium alloys: Ti-6Mo-3Fe-5Ta, Ti-4Mo-2Fe-5Ta and Ti-6Mo-3Fe-5Zr-5Hf alloys. The non-toxicity of the specially designed titanium alloys compared with osteoblastic cells has been ascertained using MTT and RN tests. In addition, phase transformations upon thermal processing have been investigated, with comparison with a well-defined beta titanium alloy. Optimum thermal processing windows (above 550 degrees C) have been designed to generate a stable and nanostructured alpha phase from the isothermal omega phase that precipitates in a low temperature range (150-350 degrees C). The generation of such nanostructured microstructures should provide a promising opportunity to investigate tissue-biomaterial interactions at the scale of biomolecules such as proteins.

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