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Phase transformations in a metastable beta Zr–12Nb alloy were investigated by high-energy X-ray diffraction (HEXRD) measured simultaneously with thermal expansion in situ during linear heating from room temperature to 800 °C. Complementary in-situ methods of electrical resistance and differential scanning calorimetry, which were performed using the same heating conditions as in the HEXRD experiment, provided additional information on the transformation sequence occurring in the Zr–12Nb alloy. Two bcc phases with a different lattice parameter, βZr and βNb, were observed in the investigated temperature range and identified using the phase diagram of the Zr–Nb system. In the initial solution-treated condition, metastable βZr phase and athermal ω particles are present in the material. At about 300 °C, Nb-rich βNb phase starts to form in the material and the original βZr phase gradually disappears. Ex-situ observations of the microstructure using transmission electron microscopy revealed a cuboidal shape of the ω particles, which is related to a relatively large misfit between the ω and β phases. At 560 °C, ω solvus was observed, identified by an abrupt dissolution of ω particles which was followed by growth of the α phase.

Compositionally graded Ti(4–12 wt% Mo) alloys were successfully prepared by laser directed energy deposition (L-DED) using two hoppers from Ti and Ti-15Mo master alloy powders. Detailed SEM, EDS and XRD analysis reveals the variation of the microstructure and consequently explains the evolution of the microhardness with the Mo concentration. High laser power is required to dissolve Ti-15Mo particles, to improve the homogeneity of the material at the scale of particle size, and to achieve a smooth linear gradient of the chemical composition. In the bottom part of the samples, the microstructure consists of elongated beta grains of the length of several mm containing big α-Ti laths. With increasing Mo concentration, the volume fraction of α phase decreases. Starting from the composition of about 9 wt% Mo the presence of ω phase was detected. Microhardness values span over a wide range of 270–550 HV and are affected by phase composition. The highest values of microhardness are achieved at around 10 wt% of Mo. However, phase composition and microhardness depend also on the utilized laser power and position in the sample determining the cooling rates. L-DED is capable of producing functionally graded materials (FGM) on the basis of metastable β-Ti alloys providing large variations of mechanical properties within a single sample/product.

Ti-8.5Mo (wt%) alloy was prepared by laser directed energy deposition (L-DED) from the mixture of cp-Ti and Ti-15Mo powder in the ratio of 50:50 using constant laser power of 600 W. Microstructure of as-printed material was characterized by microhardness mapping, light and scanning electron microscopy employing EDS technique and local X-ray diffraction measurements. In particular, the influence of the baseplate preheating to 500 °C on microstructure evolution was determined. The microstructure of the as-deposited samples consists of columnar grains orientated parallel to the building direction. Volume fraction of α, β and ω phases, and consequently also microhardness, vary for different positions within the sample due to different thermal history during the printing process. Bottom part of the sample contains increased fraction of α phase due to longer exposure to temperatures favorable for α phase precipitation. Preheating of the baseplate provides additional thermodynamic stabilization of the α phase. Numerical model, predicting the temperature evolution in each layer of the sample during deposition and consequently the ultimate phase composition, was developed. The results obtained from the model are consistent with the experimentally observed phase transformations.

Low-alloyed zirconium alloys are widely used in nuclear applications due to their low neutron absorption cross-section. These alloys, however, suffer from limited strength. Well-established guidelines for the development of Ti alloys were applied to design new two-phase ternary Zr alloys with improved mechanical properties. Zr-4Sn-4Nb and Zr-8Sn-4Nb alloys have been manufactured by vacuum arc melting, thermo-mechanically processed by annealing, forging, and aging to various microstructural conditions and thoroughly characterized. Detailed Scanning electron microscopy (SEM) analysis showed that the microstructural response of the alloys is rather similar to alpha + beta Ti alloys. Duplex microstructure containing primary alpha phase particles surrounded by lamellar alpha + beta microstructure can be achieved by thermal processing. Mechanical properties strongly depend on the previous treatment. Ultimate tensile strength exceeding 700 MPa was achieved exceeding the strength of commercial Zr alloys for nuclear applications by more than 50%. Such an improvement in strength more than compensates for the increased neutron absorption cross-section. This study aims to exploit the potential of alpha + beta Zr alloys for nuclear applications.

Recent years have witnessed much progress in medical device manufacturing and the needs of the medical industry urges modern nanomaterials science to develop novel approaches for improving the properties of existing biomaterials. One of the ways to enhance the material properties is their nanostructuring by using severe plastic deformation (SPD) techniques. For medical devices, such properties include increased strength and fatigue life, and this determines nanostructured Ti and Ti alloys to be an excellent choice for the engineering of implants with improved design for orthopedics and dentistry. Various reported studies conducted in this field enable the fabrication of medical devices with enhanced functionality. This paper reviews recent development in the field of nanostructured Ti-based materials and provides examples of the use of ultra-fine grained Ti alloys in medicine.

Beta titanium alloy Ti-35Nb-6Ta-7Zr-0.7O (wt%) was developed as a material intended for the manufacturing of a stem of a hip joint replacement. This alloy contains only biocompatible elements and possesses a very high yield strength already in the cast condition (900 MPa). However, the porosity, large grain size and chemical inhomogeneity reduce the fatigue performance below the limits required for utilization in the desired application. Two methods of hot working, die forging and hot rolling, were used for processing of this alloy. Microstructural evolution, tensile properties and fatigue performance of the hot worked material were investigated and compared to the cast material. Microstructural observations revealed that porosity is removed in all hot-worked conditions and the grain size is significantly reduced when the area reduction exceeds 70%. Static tensile properties were improved by both processing methods and ultimate tensile strength (UTS) of 1200 MPa was achieved. Fatigue results were more reproducible in the hot rolled material due to better microstructural homogeneity, but forging leads to an improved fatigue performance. Fatigue limit of 400 MPa was achieved in the die-forged condition after 70% of area reduction and in the hot rolled condition after 86% of area reduction.

A transformation pathway during thermal treatment of metastable β Ti-15Mo alloy was investigated by in situ neutron diffraction. The evolution of individual phases α , β , and ω was investigated during linear heating with two heating rates of 1.9 ∘ C / min and 5 ∘ C / min and during aging at 450 ∘ C . The results showed that with a sufficient heating rate (5 ∘ C / min in this case), the ω phase dissolves before the α phase forms. On the other hand, for the slower heating rate of 1.9 ∘ C / min , a small temperature interval of the coexistence of the α and ω phases was detected. Volume fractions and lattice parameters of all phases were also determined.

A composite of powders of semi-Heusler ferromagnetic shape memory and pure titanium was successfully prepared by spark plasma sintering at the temperature of 950 °C. Sintering resulted in the formation of small precipitates and intermetallic phases at the heterogeneous interfaces. Various complementary experimental methods were used to fully characterize the microstructure. Imaging methods including transmission and scanning electron microscopy with energy dispersive X-ray spectroscopy revealed a position and chemical composition of individual intermetallic phases and precipitates. The crystalline structure of the phases was examined by a joint refinement of X-ray and neutron diffraction patterns. It was found that Co 38 Ni 33 Al 29 decomposes into the B2-(Co,Ni)Al matrix and A1-(Co,Ni,Al) particles during sintering, while Al, Co and Ni diffuse into Ti forming an eutectic two phase structure with C9-Ti 2 (Co,Ni) precipitates. Complicated interface intermetallic structure containing C9-Ti 2 (Co,Ni), B2-(Co,Ni)Ti and L2 1 -(Co,Ni)(Al,Ti) was completely revealed. In addition, C9-Ti 2 (Co,Ni) and A1-(Co,Ni,Al) precipitates were investigated by an advanced method of small angle neutron scattering. This study proves that powder metallurgy followed by spark plasma sintering is an appropriate technique to prepare bulk composites from very dissimilar materials.

Low-modulus biomedical beta titanium alloys often suffer from low strength which limits their use as load-bearing orthopaedic implants. In this study, twelve different Ti-Nb-Zr-Ta based alloys alloyed with Fe, Si and O additions were prepared by arc melting and hot forging. The lowest elastic modulus (65GPa) was achieved in the benchmark TNTZ alloy consisting only of pure β phase with low stability due to the 'proximity' to the β to α'' martensitic transformation. Alloying by Fe and O significantly increased elastic modulus, which correlates with the electrons per atom ratio (e/a). Sufficient amount of Fe/O leads to increased yield stress, increased elongation to fracture and also to work hardening during deformation. A 20% increase in strength and a 20% decrease in the elastic modulus when compared to the common Ti-6Al-4V alloy was achieved in TNTZ-Fe-Si-O alloys, which proved to be suitable for biomedical use due to their favorable mechanical properties., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

Beta titanium alloys are promising materials for load-bearing orthopaedic implants due to their excellent corrosion resistance and biocompatibility, low elastic modulus and moderate strength. Metastable beta-Ti alloys can be hardened via precipitation of the alpha phase; however, this has an adverse effect on the elastic modulus. Small amounts of Fe (0-2 wt.%) and Si (0-1 wt.%) were added to Ti-35Nb-7Zr-6Ta (TNZT) biocompatible alloy to increase its strength in beta solution treated condition. Fe and Si additions were shown to cause a significant increase in tensile strength and also in the elastic modulus (from 65 GPa to 85 GPa). However, the elastic modulus of TNZT alloy with Fe and Si additions is still much lower than that of widely used Ti-6Al-4V alloy (115 GPa), and thus closer to that of the bone (10-30 GPa). Si decreases the elongation to failure, whereas Fe increases the uniform elongation thanks to increased work hardening. Primary human osteoblasts cultivated for 21 days on TNZT with 0.5Si+2Fe (wt.%) reached a significantly higher cell population density and significantly higher collagen I production than cells cultured on the standard Ti-6Al-4V alloy. In conclusion, the Ti-35Nb-7Zr-6Ta-2Fe-0.5Si alloy proves to be the best combination of elastic modulus, strength and also biological properties, which makes it a viable candidate for use in load-bearing implants., (Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.)

This study investigated the properties of Ti-6Al-4V alloy after surface treatment by the electric discharge machining (EDM) process. The EDM process with high peak currents proved to induce surface macro-roughness and to cause chemical changes to the surface. Evaluations were made of the mechanical properties by means of tensile tests, and of surface roughness for different peak currents of the EDM process. The EDM process with peak current of 29 A was found to induce sufficient surface roughness, and to have a low adverse effect on tensile properties. The chemical changes were studied by scanning electron microscopy equipped with an energy dispersive X-ray analyser (EDX). The surface of the benchmark samples was obtained by plasma-spraying a titanium dioxide coating. An investigation of the biocompatibility of the surface-treated Ti-6Al-4V samples in cultures of human osteoblast-like MG 63 cells revealed that the samples modified by EDM provided better substrates for the adhesion, growth and viability of MG 63 cells than the TiO2 coated surface. Thus, EDM treatment can be considered as a promising surface modification to orthopaedic implants, in which good integration with the surrounding bone tissue is required., (Copyright © 2011 Elsevier Ltd. All rights reserved.)

Three different microstructures--equiaxed, bi-modal and coarse lamellar--are prepared from Ti-6Al-4V alloy. Electric discharge machining (EDM) with a high peak current (29 A) is performed in order to impose surface roughness and modify the chemical composition of the surface. Detailed scanning electron microscopy (SEM) investigation revealed a martensitic surface layer and subsurface heat affected zone (HAZ). EDX measurements showed carbon enriched remnants of the EDM process on the material surface. Rotating bending fatigue tests are undertaken for EDM processed samples for all three microstructures and also for electropolished-benchmark-samples. The fatigue performance is found to be rather poor and not particularly dependent on microstructure. The bi-modal microstructure shows a slightly superior high cycle fatigue performance. This performance can be further improved by a suitable heat treatment to an endurance limit of 200 MPa., (Copyright © 2011 Elsevier Ltd. All rights reserved.)

Ti-6Al-4V hour-glass shaped rotating beam specimens with duplex microstructure were processed by electric discharge machining (EDM). A comparatively high peak current of 29A was utilized in order to increase surface roughness for improved osteointegration. High cycle fatigue (HCF) tests were performed in rotating beam loading (R=-1) on these EDM specimens and results were compared with electrolytically polished specimens serving as reference. As expected, the HCF performance of EDM specimens was inferior to the electrolytically polished specimens. A detailed study of fatigue crack nucleation and microcrack growth was carried out on failed specimens by SEM. The poor HCF strength of EDM specimens is explained by early crack nucleation due to the high notch sensitivity of Ti-6Al-4V. In addition, process-induced residual tensile stresses and microstructural effects may also account for the drastic loss in HCF performance relative to the electropolished baseline., (Copyright © 2010 Elsevier Ltd. All rights reserved.)