Compressibility of a Ti-based alloy with varying amounts of surfactant prepared by high-energy ball milling

The combined effects of varying amounts of surfactant (ethylene bis-stearamide; EBS) and milling time on the compressibility of ball-milled Ti-10Nb-3Mo (wt.%) alloy were investigated. Ball milling process was performed on the elemental powders with different amounts of EBS (0-3. wt.%) for 5 and 10. h, and the ball-milled powders were consolidated by a uniaxial cold pressing in the range of 500-1100. MPa. Results indicated that the addition of surfactant in ball milling process lead to significant changes in particle packing density. The relative density was higher for powders ball milled with larger amounts of EBS and for the shorter milling time. The compressibility of powders was examined by the compaction equation developed by Panelli and Ambrosio Filho. The densification parameter (A) increased with the increasing amount of EBS, and decreased with increasing milling time.

Microstructure and mechanical properties of Ti-15Zr alloy used as dental implant material

Ti-Zr alloys have recently started to receive a considerable amount of attention as promising materials for dental applications. This work compares mechanical properties of a new Ti-15Zr alloy to those of commercially pure titanium Grade4 in two surface conditions - machined and modified by sand-blasting and etching (SLA). As a result of significantly smaller grain size in the initial condition (1-2µm), the strength of Ti-15Zr alloy was found to be 10-15% higher than that of Grade4 titanium without reduction in the tensile elongation or compromising the fracture toughness. The fatigue endurance limit of the alloy was increased by around 30% (560MPa vs. 435MPa and 500MPa vs. 380MPa for machined and SLA-treated surfaces, respectively). Additional implant fatigue tests showed enhanced fatigue performance of Ti-15Zr over Ti-Grade4.

Processing and mechanical properties of porous titanium-niobium shape memory alloy for biomedical applications

Ti-26 at.%Nb (hereafter Ti-26Nb) alloy foams were fabricated by space-holder sintering process. The porous structures of the foams were characterized by scanning electron microscopy (SEM). The mechanical properties of the Ti-26Nb foam samples were investigated using compressive test. Results indicate that mechanical properties of Ti-26Nb foam samples are influenced by foam porosity. The plateau stresses and elastic moduli of the foams under compression decrease with the increase of their porosities. The plateau stresses and elastic moduli are measured to be from 10~200 MPa and 0.4~5.0 GPa for the Ti-26Nb foam samples with porosities ranged from 80~50 %, respectively.

Precipitate characterisation of an advanced high-strength low-alloy (HSLA) steel using atom probe tomography

Increased fuel economy, combined with the need for the improved safety has generated the development of new hot-rolled high-strength low-alloy (HSLA) and multiphase steels such as dual-phase or transformation-induced plasticity steels with improved ductility without sacrificing strength and crash resistance. However, the modern multiphase steels with good strength-ductility balance showed deteriorated stretch-flangeability due to the stress concentration region between the soft ferrite and hard martensite phases [1]. Ferritic, hot-rolled steels can provide good local elongation and, in turn, good stretch-flangeability [2]. However, conventional HSLA ferritic steels only have a tensile strength of not, vert, similar600 MPa, while steels for the automotive industry are now required to have a high tensile strength of not, vert, similar780 MPa, with excellent elongation and stretch-flangeability [1]. This level of strength and stretch-flangeability can only be achieved by precipitation hardening of the ferrite matrix with very fine precipitates and by ferrite grain refinement. It has been suggested that Mo [3] and Ti [4] should be added to form carbides and decrease the coiling temperature to 650 °C since only a low precipitation temperature can provide the precipitation refinement [4]. These particles appeared to be (Ti, Mo)C, with a cubic lattice and a parameter of 0.433 nm, and they were aligned in rows [4]. It was reported [4] that the formation of these very fine carbides led to an increase in strength of not, vert, similar300 MPa. However, the detailed analysis of these particles has not been performed to date due to their nanoscale size. The aim of this work was to carry out a detailed investigation using atom probe tomography (APT) of precipitates formed in hot-rolled low-carbon steel containing additions Ti and Mo.

The investigated low-carbon steel, containing Fe–0.1C–1.24Mn–0.03Si–0.11Cr–0.11Mo–0.09Ti–0.091Al at.%, was produced by hot rolling. The processing route has been described in detail elsewhere [5] European Patent Application, 1616970 A1, 18.01.2006.[5]. The microstructure was characterised by transmission electron microscopy (TEM) on a Philips CM 20, operated at 200 kV using thin foil and carbon replica techniques. Qualitative energy dispersive X-ray spectroscopy (EDXS) was used to analyse the chemical composition of particles. The atomic level of particle characterisation was performed at the University of Sydney using a local electrode atom probe [6]. APT was carried out using a pulse repetition rate of 200 kHz and a 20% pulse fraction on the sample with temperature of 80 K. The extent of solute-enriched regions (radius of gyration) and the local solute concentrations in these regions were estimated using the maximum separation envelope method with a grid spacing of 0.1 nm [7]. A maximum separation distance between the atoms of interest of dmax = 1 nm was used.

The microstructure of the steel consisted of two types of fine ferrite grains: (i) small recrystallised grains with an average grain size of 1.4 ± 0.2 μm; and (ii) grains with a high dislocation density (5.8 ± 1.4 × 1014 m−2) and an average grain size of 1.9 ± 0.1 μm in thickness and 2.7 ± 0.1 μm in length (Fig. 1a). Some grains with high dislocation density displayed an elongated shape with Widmanstätten side plates and also the formation of cells and subgrains (Fig. 1a). The volume fraction of recrystallised grains was 34 ± 8%.

TiNi shape memory alloy foams synthesized by spacer sintering and their properties

Titanium (Ti) and nickel (Ni) elemental powders were blened by ball milling and the ball milled powders were employed to fabricate NiNi shape memory alloy (SMA) foams by space sintering. Effect of ball milling time on phase constitutes of the sintered TiNi alloy foams was studied by X-ray diffraction (XRD) analysis.Scanning election microscopy (SEM) was used to characterize the porous structure, and compressive tests were carried out to evaluate the mechanical properties of the foams. Results indicate the porosities of the TiNi alloy foams can be controlled by using the spacer sincering method, and the porosities show a significant effect on the mechanical prperties and shape memory effect (SME).

Effect of surface roughness of Ti, Zr, and TiZr on apatite precipitation from simulated body fluid

Some of the critical properties for a successful orthopedic or dental implant material are its biocompatibility and bioactivity. Pure titanium (Ti) and zirconium (Zr) are widely accepted as biocompatible metals, due to their non-toxicity. While the bioactivity of Ti and some Ti alloys has been extensively investigated, there is still insufficient data for Zr and titanium-zirconium (TiZr) alloys. In the present study, the bioactivity, that is, the apatite forming ability on the alkali and heat treated surfaces of Ti, Zr, and TiZr alloy in simulated body fluid (SBF), was studied. In particular, the effect of the surface roughness characteristics on the bioactivity was evaluated for the first time. The results indicate that the pretreated Ti, Zr and TiZr alloy could form apatite coating on their surfaces. It should be noted that the surface roughness also critically affected the bioactivity of these pretreated metallic samples. A surface morphology with an average roughness of approximately 0.6 microm led to the fastest apatite formation on the metal surfaces. This apatite layer on the metal surface is expected to bond to the surrounding bones directly after implantation.

Synthesis of Ti–Sn–Nb alloy by powder metallurgy

The microstructural evolution and characteristics of the Ti–16Sn–4Nb powder particles and bulk alloys sintered from the powders ball-milled for various periods of time were studied. Results indicated that ball milling to 8 h led to the development of a supersaturated hcp α-Ti and partial amorphous phase due to the solid solution of Sn and Nb into Ti lattice. The bulk Ti–16Sn–4Nb alloy made from the powders ball milled for a short time, up to 2 h, exhibited a primary α and a Widmanstätten structure consisting of interlaced secondary α and β. With an increase in ball milling time up to 10 h, the microstructure evolved into a fine β phase dispersed homogeneously within α phase matrix. The microhardness values of the bulk alloy in both α- and β-phases increased with the increasing of the ball milling time and reached a plateau value at 8 h and longer, i.e. 687 and 550 HV for α- and β-phases, respectively. Likewise, the microhardness of the α phases was always higher than that of the β phases in the bulk alloys made from the powders ball milled for the same milling time.

Influence of porosity on shape memory behavior of porous TiNi shape memory alloy

Porous Ti-50.5at.%Ni shape memory alloy (SMA) samples with a range of  porosities were prepared by spacer sintering. The porous structure of the alloy was examined using scanning electron microscopy (SEM). The phase constituents of the porous TiNi alloy were determined by X-ray diffraction (XRD). The shape memory behavior of the porous TiNi alloy was investigated using loading–unloading compression tests. Results indicate that the porous TiNi alloy exhibits superelasticity and the recoverable strain by the superelasticity decreases with the increase of porosity. After a prestrain of 7%, the superelastically recovered strains for the porous TiNi alloy samples with porosities of 46%, 59%, 69% and 77% are 2.0%, 1.8%, 1.5% and 1.3%, respectively. The pores in the TiNi alloy samples cause stress/strain concentration, as well as crack initiation, which adversely affect the shape memory behavior of the porous TiNi alloy.

The effect of hydrogenation on the ECAP compaction of Ti–6Al–4V powder and the mechanical properties of compacts

The effect of hydrogen content on the compaction of Ti–6Al–4V powder at low temperatures, namely 500 °C, using equal channel angular pressing (ECAP) with back pressure has been investigated. The properties of the compacts before and after a heat treatment and de-hydrogenation cycle have been determined. Compaction of powder by ECAP (500 °C and 260 MPa) has shown maximum levels of relative density of 99.3% and 99.4% when charged with 0.05–0.1 wt.% and 0.61–0.85 wt.% of hydrogen, respectively. After the de-hydrogenation heat treatment the diffusion bonding between individual powder particles was completed and the microstructure was altered, depending on the level of hydrogen content. Two local maxima of 99.2% and 98.1% were observed in the measured density of consolidated compacts for hydrogen contents between 0.05 wt.% and 0.1 wt.% and between 0.61 wt.% and 0.85 wt.%, respectively. However, the mechanical properties of the compacts within these two ranges of hydrogen content were significantly different due to a difference in the observed microstructure. An exceptionally high ductility of 29%, in combination with a relatively high strength of ~560 MPa, was measured in a shear punch test on specimens which had a prior hydrogen level of 0.05 wt.% before the heat treatment. It was shown that material consolidated from powder hydrogenated to low levels of hydrogen before compaction has the potential to offer substantial improvements in mechanical properties after a suitable heat treatment.

In vitro cytotoxicity of binary TI alloys for bone implants

Interest in using titanium (Ti) alloys as load-bearing implant materials has increased due to their high strength to weight ratio, lower elastic modulus, and superior biocompatibility and enhanced corrosion resistance compared to conventional metals such as stainless steel and Co-Cr alloys. In the present study, the in vitro cytotoxicity of five binary titanium alloys, Ti15Ta, Ti15Nb, Ti15Zr, Ti15Sn and Ti15Mo, was assessed using human osteosarcoma cell line, SaOS-2 cells. The Cell proliferation and viability were determined, and cell adhesion and morphology on the surfaces of the binary Ti alloys after cell culture were observed by SEM. Results indicated that the Ti binary alloys of Ti15Ta, Ti15Nb and Ti15Zr exhibited the same level of excellent biocompatibility; Ti15Sn alloy exhibited a moderate biocompatibility while Ti15Mo alloy exhibited a moderate cytotoxicity. The SaOS-2 osteoblast-like cells had flattened and spread across the surfaces of the Ti15Ta, Ti15Nb, Ti15Zr and Ti15Sn groups; however, the cell shapes on the Ti15Mo alloy was shrinking and unhealthy. These results indicated that the Mo contents should be limited to a certain level in the design and development of new Ti alloys for implant material applications.

Ti6Ta4Sn alloy and subsequent scaffolding for bone tissue engineering

Porous titanium (Ti) and titanium alloys are promising scaffold biomaterials for bone tissue engineering, because they have the potential to provide new bone tissue ingrowth abilities and low elastic modulus to match that of
natural bone. In the present study, a new highly porous Ti6Ta4Sn alloy scaffold with the addition of biocompatible alloying elements (tantalum (Ta) and tin (Sn)) was prepared using a space-holder sintering method. The
strength of the Ti6Ta4Sn scaffold with a porosity of 75% was found to be significantly higher than that of a pure Ti scaffold with the same porosity. The elastic modulus of the porous alloy can be customized to match that of
human bone by adjusting its porosity. In addition, the porous Ti6Ta4Sn alloy exhibited an interconnected porous structure, which enabled the ingrowth of new bone tissues. Cell culture results revealed that human SaOS₂
osteoblast-like cells grew and spread well on the surfaces of the solid alloy, and throughout the porous scaffold. The surface roughness of the alloy showed a significant effect on the cell behavior, and the optimum surface
roughness range for the adhesion of the SaOS2 cell on the alloy was 0.15 to 0.35 mm. The present study illustrated the feasibility of using the porous Ti6Ta4Sn alloy scaffold as an orthopedic implant material with a special
emphasis on its excellent biomechanical properties and in vitro biocompatibility with a high preference by osteoblast-like cells.

Bioactive hydroxyapatite coating on titanium-niobium alloy through a sol-gel process

Hydroxyapatite (HA) was coated on the surface of a titanium-niobium (Ti-Nb) alloy by a sol-gel process. Triethyl phosphite and calcium nitrate were used as the phosphorus (P) and calcium (Ca) precursors respectively to prepare a Ca/P sol solution. The Ti-Nb alloy was dip-coated in the sol and heated at 600°C for 30 minutes. X-ray diffraction (XRD) analysis indicated the major phase constituent of the coating after heat treatment was HA. Scanning electron microscopy (SEM) observation showed that a few cracks were distributed on the HA coating. The in-vitro bioactivity of the HA coated Ti-Nb alloy was assessed using a cell culture of SaOS-2 osteoblast-like cells. The density of cell attachment was determined by MTT assay; the cell morphology was observed by SEM. Results indicated that the density of cell attachment on the surface of the Ti-Nb alloy was significantly increased by HA coating. Cell morphology observation showed that cells attached, spread and grew well on the HA coated surface. It can be concluded that the HA coating improved the in-vitro bioactivity of Ti-Nb alloy effectively.

Preparation of bioactive porous titanium-molybdenum alloy through powder metallurgy

Porous Ti-Mo alloy samples with different porosities from 52% to 72% were successfully fabricated by the space-holder sintering method. The pore size of the porous Ti-Mo alloy samples were ranged from 200 to 500 μm. The plateau stress and elastic modulus of the porous Ti-Mo alloy samples increases with the decreasing of the porosity. Moreover, an apatite coating on the Ti-Mo alloy after an alkali and heat treatment was obtained through soaking into a simulated body fluid (SBF). The porous Ti-Mo alloy provides promising potential for new implant materials with new bone tissue ingrowth ability, bioactivity and mechanical properties mimicking those of natural bone.

Effect of NbC and TiC precipitation on shape memory in an iron-based alloy

This paper examines the effects of TiC and NbC precipitation and prior cold rolling on the shape memory behaviour of an iron-based alloy. A precipitate-free alloy was used as a reference to investigate the relative contributions of prior-deformation and precipitation on shape memory. Heat treatment of the Nb- and Ti-containing alloys at 700 °C and 800 °C resulted in carbide precipitates between 120 nm and 220 nm in diameter. Bend testing of these samples showed a marginal increase in shape memory compared to the precipitate-free alloy. Under these conditions TiC precipitation exhibited slightly better shape memory than for NbC. However, this small increase was over-shadowed by the marked increase in shape memory that can be produced by subjecting the alloys to cold rolling followed by recovery annealing. When processed in this way, fine carbides are formed in the Ti- and Nb-containing alloys during the heat treatment. For particles >25 nm in diameter the shape memory is unaffected, but, it was found that small <5 nm particles have a detrimental effect on shape memory due to pinning of the martensite plates, thereby inhibiting their reversion to austenite. The optimum shape memory was observed in the precipitate-free alloy after cold rolling and recovery annealing.

Porous TiNbZr alloy scaffolds for biomedical applications

In the present study, porous Ti–10Nb–10Zr alloy scaffolds with different porosities were successfully fabricated by a ‘‘space-holder” sintering method. By the addition of biocompatible alloying elements the porous TiNbZr scaffolds achieved significantly higher strength than unalloyed Ti scaffolds of the same porosity. In particular, the porous TiNbZr alloy with 59% porosity exhibited an elastic modulus and plateau stress of 5.6 GPa and 137 MPa, respectively. The porous alloys exhibited excellent ductility during compression tests and the deformation mechanism is mainly governed by bending and buckling of the struts. Cell cultures revealed that SaOS2 osteoblast-like cells grew on the surface and inside the pores and showed good spreading. Cell viability for the porous scaffold was three times higher than the solid counterpart. The present study has demonstrated that the porous TiNbZr alloy scaffolds are promising scaffold biomaterials for
bone tissue engineering by virtue of their appropriate mechanical properties, highly porous structure and excellent biocompatibility.