Javier Andres Muñoz Chaves

Influence of phase transformations on dynamical elastic modulus and anelasticity of beta Ti-Nb-Fe alloys for biomedical applications

Recent studies in materials for biomedical applications have focused on β-titanium alloys that are highly biocompatible, free of toxic elements and with an elastic modulus close to that of human bone (10-40 GPa). Beta Ti-xNb-3Fe (x=10, 15, 20 and 25 wt%) alloys were obtained by rapid solidification and characterized by anelastic relaxation measurements at temperatures between 140 K and 770 K, using a free-decay elastometer, as well as analysis by Differential Scanning Calorimetry (DSC), X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The observed stabilization of the β-phase with rising Nb content was linked to the strength of the relaxation peak around 570 K. The phase transformations detected in the anelastic relaxation spectra agreed with those observed in the DSC curves. However, the results from anelastic relaxation spectra provide more detailed information about the kinetics of phase transformations. At temperatures between 140 K and 300 K, there was an indication of a reversible transformation in the alloys studied. The elastic modulus measurements showed a hardening of the material, between 400 K and 620 K, related to the ω-phase precipitation. However, the starting temperature of ω-phase precipitation was clearly influenced by the Nb content, showing a shift to high temperature with increasing percentage of Nb. At temperatures above 620 K, a fall was observed in the dynamical elastic modulus, accompanied by a relaxation peak centered at 660 K, which was attributed to the growing α-phase arising from the ω-phase, which acts as a nucleation sites or from the decomposition of the metastable β-phase. XRD patterns confirmed the formation of β, α and ω phases after mechanical relaxation measurements. A predominant β phase with dendritic morphology was observed, which became more stable with 25 wt% Nb. The lowest elastic modulus was of 65 GPa obtained in the Ti-25Nb-3Fe alloy, representing a good low value for a β-Ti alloy with a relatively low addition of β stabilizing elements (Nb and Fe).

Dynamical Elastic Moduli of the Ti-13Nb-13Zr biomaterial alloy by mechanical spectroscopy

Dynamical Elastic Moduli of the Ti-13Nb-13Zr biomaterial alloy were obtained using the mechanical spectroscopy technique. The sample with heat treatment at 1170K for 30 minutes and water quenched with subsequent aging treatment at 670 K for 3 hours (TNZ + WQ + 670 K/3 h), was characterized through decay of free oscillations of the sample in the flexural vibration mode. The spectra of anelastic relaxation (internal friction and frequency) in the temperature range from 300 K to 625 K not revealed the presence of relaxation process. As shown in the literature, the hcp structure usually does not exhibit any relaxation due to the symmetry of the sites in the crystalline lattice, but if there is some relaxation, this only occurs in special cases such as low concentration of zirconium or saturation of the stoichiometric ratio of oxygen for zirconium. Dynamical elastic modulus obtained for TNZ + WQ + 670 K/3 h alloy was 87 GPa at room temperature, which is higher than the value for Ti-13Nb-13Zr alloy (64 GPa) of the literature. This increment may be related to the change of the proportion of α and β phases. Besides that, the presence of precipitates in the alloy after aging treatment hardens the material and reduces its ductility.

Elastic Behavior of the Ti-13Nb-13Zr Alloy Obtained by Anelastic Spectroscopy

Measurements of anelastic relaxation (internal friction and frequency) as a function of temperature were carried out in samples of Ti-13Nb-13Zr using two experimental apparatus: Flexural Vibration of the first tone of samples in Acoustic Elastometer System (Vibran Technology®) operating in a kilohertz bandwidth, and Torsional Vibration of the samples in Kê-type Torsion Pendulum operating in a hertz bandwidth. Experimental spectra of anelastic relaxation were determined in the temperature range from 300 K to 450 K for a heating rate of 1K/min under pressure of 10-5 Torr, in both apparatus. The results show a relaxation structure strongly dependent on the microstructure of the material. The dynamical elastic modulus (E) of Ti-13Nb-13Zr alloy can be determined by flexural vibrations by frequency (f) measurements (f  E1/2). The anelastic relaxation spectrum of Ti-13Nb-13Zr alloy was a function of temperature obtained by torsional vibrations, not revealing the presence of interstitial solutes in solid solution in the temperature range of measurements.

Study on Cu48Zr43Al9 and Cu54Zr40Al6 Amorphous Matrix Alloys by Mechanical Spectroscopy

Anelastic properties of Bulk Metallic Glasses (BMG) were studied by mechanical spectroscopy using a flexural vibration apparatus. BMG’s samples, with nominal composition Cu48Zr43Al9 and Cu54Zr40Al6, were produced by skull push-pull casting technique in rectangular cavity cooper mold. In both samples, the differential scanning calorimeter patterns have evidenced the presence of amorphous structure, although the X-ray diffraction for Cu48Zr43Al9 composition has shown a heterogeneous microstructure embedded in the amorphous matrix. Anelastic relaxation spectra were obtained using an acoustic elastometer system with vibration frequency in the kilohertz bandwidth, a heating rate of 1 K/min, vacuum greater than 10-5 mBar in the temperature range of 300 K to 620 K. In the flexural apparatus, an acoustic elastometer system, the internal friction (energy loss) and the elastic modulus were obtained by free decay of vibrations and by the squared of the oscilation frequency, respectively. Internal friction spectra were not reproducible among the measurements, which may imply atomic rearrangement in the samples due to consecutive heating. Normalized elastic modulus data showed distinct behavior from the first to the other measurements evidencing irreversible microstructural alterations in the samples possibly associated with mechanical relaxation due to the motion of atoms or clusters in the glassy state.

Mechanical Spectroscopy Study on Cu53.5Zr42Al4.5 Alloy

This study consists of the characterization of the anelastic properties of a Bulk Metallic Glasses (BMG) by mechanical spectroscopy, which can be defined as an energy absorption technique. The equipment used was the acoustic elastometer system, the anelastic relaxation spectra were carried out with a heating rate of 1 K/min and vacuum better than 10-5 torr, in the temperature range of 300 K to 640 K. The amorphous sample studied, with nominal composition of Cu53.5Zr42Al4.5, was processed by skull push-pull casting technique in a rectangular cavity cooper mould. Differential scanning calorimeter (DSC) curves have evidenced the amorphous structure although the X-ray diffraction (XDR) pattern has indicated a heterogeneous microstructure with amorphous matrix and some metaestable nanocrystalline phases which have not been identified yet. The dynamical elastic modulus of this alloy (between 54 GPa and 58 GPa at room temperature) and internal friction patterns as temperature function implied an increase of the crystalline phase during the measurements. This effect was confirmed with new X-ray diffraction measurements after the internal friction experiments.