Petr Harcuba

Surface treatment by electric discharge machining of Ti-6Al-4V alloy for potential application in orthopaedics.

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.

The effect of microstructure on fatigue performance of Ti–6Al–4V alloy after EDM surface treatment for application in orthopaedics

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.

Newly developed Ti-Nb-Zr-Ta-Si-Fe biomedical beta titanium alloys with increased strength and enhanced biocompatibility.

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.

Fatigue endurance of Ti-6Al-4V alloy with electro-eroded surface for improved bone in-growth.

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.

Innovative surface modification of Ti–6Al–4V alloy with a positive effect on osteoblast proliferation and fatigue performance

A novel approach of surface treatment of orthopaedic implants combining electric discharge machining (EDM), chemical milling (etching) and shot peening is presented in this study. Each of the three techniques have been used or proposed to be used as a favourable surface treatment of biomedical titanium alloys. But to our knowledge, the three techniques have not yet been used in combination. Surface morphology and chemistry were studied by scanning electron microscopy and X-ray photoelectron spectroscopy, respectively. Fatigue life of the material was determined and finally several in-vitro biocompatibility tests have been performed. EDM and subsequent chemical milling leads to a significant improvement of osteoblast proliferation and viability thanks to favourable surface morphology and increased oxygen content on the surface. Subsequent shot-peening significantly improves the fatigue endurance of the material. Material after proposed combined surface treatment possesses favourable mechanical properties and enhanced osteoblast proliferation. EDM treatment and EDM with shot peening also supported early osteogenic cell differentiation, manifested by a higher expression of collagen type I. The combined surface treatment is therefore promising for a range of applications in orthopaedics.

Ordered array of ω particles in β-Ti matrix studied by small-angle X-ray scattering

Abstract Nanosized particles of ω phase in a β -Ti alloy were investigated by small-angle X-ray scattering using synchrotron radiation. We demonstrated that the particles are spontaneously weakly ordered in a three-dimensional cubic array along the 〈 1 0 0 〉 -directions in the β -Ti matrix. The small-angle scattering data fit well to a three-dimensional short-range-order model; from the fit we determined the evolution of the mean particle size and mean distance between particles during ageing. The self-ordering of the particles is explained by elastic interaction between the particles, since the relative positions of the particles coincide with local minima of the interaction energy. We performed numerical Monte Carlo simulation of the particle ordering and we obtained a good agreement with the experimental data.

Twin domain imaging in topological insulator Bi2Te3 and Bi2Se3 epitaxial thin films by scanning X-ray nanobeam microscopy and electron backscatter diffraction

Imaging with surface- and bulk-sensitive electron and X-ray diffraction based microscopic techniques enabled identification of the twin domain distribution of Bi2Te3 and Bi2Se3 thin films. Correlations between the surface topography and crystal orientation are established.

Observation of individual stacking faults in GaN microcrystals by x-ray nanodiffraction

X-ray nanodiffraction was used for the investigation of basal stacking faults in a-GaN microcrystallites. The method made it possible to find the positions of individual stacking faults in a chosen crystallite, and the resulting positions were compared with the observation of individual faults by electron channeling contrast in scanning electron microscopy. The x-ray diffraction data revealed that the faults occur in closely positioned pairs; the stacking faults in a pair have opposite displacement vectors.

Microstructure and high temperature deformation of an ultra-fine grained ECAP AA7075 aluminium alloy

Abstract An AA 7075 aluminium alloy with an ultra-fine grained structure was prepared through equal channel angular pressing (ECAP) at pressing temperatures TECAP of 120, 170, and 220 °C. A decrease in TECAP from 220 to 120 °C was found to lead to a more pronounced refinement of the microstructure and to worse stability of the microstructure – the onset of grain coarsening was displaced to lower temperatures. The material pressed with the highest TECAP exhibited superplastic behaviour at temperatures close to 400 °C and grain boundary sliding was identified as the dominant operating deformation mechanism. The materials prepared with both of the lower TECAP exhibited only enhanced ductility of about 200 %, however this behaviour was observed at temperatures as low as 200 °C. It was found that this “low temperature superplasticity” resulted from a combined operation of grain boundary sliding at selected grain boundaries and glide of lattice dislocations.

Growth kinetics of ω particles in β-Ti matrix studied by in situ small-angle X-ray scattering

Nucleation and growth kinetics of nanoparticles of hexagonal ω phase in a body-centered cubic β titanium matrix in single crystals of β-Ti alloys were investigated by small-angle x-ray scattering measured in-situ during ageing at various temperatures up to 450 °C. The experimental data were compared with numerical simulations based on a three-dimensional short-range order model of nanoparticle self-ordering. The x-ray contrast of the particles is caused by an inhomogeneous distribution of impurity atoms (Mo, Fe and Al), whose density profile around growing nanoparticles was simulated by solving the corresponding diffusion equation with moving boundary conditions. From the analysis of the experimental data we determined the mean distance and size of the nanoparticles and confirmed the validity of the ∝ t1/3 growth law following from the Lifshitz-Slyozov-Wagner theory. From a detailed comparison of the experimental data with simulations we also assessed the diffusion coefficient of the impurity atoms and its activation energy.