Laser and electron beam additive manufacturing methods of fabricating titanium bone implants

Additive Manufacturing (AM) methods are generally used to produce an early sample or near net-shape elements based on three-dimensional geometrical modules. To date, publications on AM of metal implants have mainly focused on knee and hip replacements or bone scaffolds for tissue engineering. The direct fabrication of metallic implants can be achieved by methods, such as Selective Laser Melting (SLM) or Electron Beam Melting (EBM). This work compares the SLM and EBM methods used in the fabrication of titanium bone implants by analyzing the microstructure, mechanical properties and cytotoxicity. The SLM process was conducted in an environmental chamber using 0.4–0.6 vol % of oxygen to enhance the mechanical properties of a Ti-6Al-4V alloy. SLM processed material had high anisotropy of mechanical properties and superior UTS (1246–1421 MPa) when compared to the EBM (972–976 MPa) and the wrought material (933–942 MPa). The microstructure and phase composition depended on the used fabrication method. The AM methods caused the formation of long epitaxial grains of the prior phase. The equilibrium phases ( + ) and non-equilibrium ’ martensite was obtained after EBM and SLM, respectively. Although it was found that the heat transfer that occurs during the layer by layer generation of the component caused aluminum content deviations, neither methods generated any cytotoxic effects. Furthermore, in contrast to SLM, the EBM fabricated material met the ASTMF136 standard for surgical implant applications.peer-reviewe

In situ alloying of NiTi : influence of laser powder bed fusion (LBPF) scanning strategy on chemical composition

NiTi alloys are widely used in different industrial and medical applications. Due to the inherent difficulty in the machining of these alloys, the use of Additive Manufacturing (AM) methods has become a popular method for their production. When working with NiTi alloys, there is a requirement on the precise control of their chemical composition, as this determines the phase transition temperatures which are responsible for their shape memory or superelastic behaviour. The high energies used in AM to melt the NiTi alloy leads to nickel evaporation, resulting in a chemical change between the batch powder and the additively manufactured part. Therefore, in AM techniques applied to different NiTi alloys, understanding the relationship between the melting strategy and nickel evaporation is crucial during the developing the desired chemical composition of the final-fabricated material. In this study, three NiTi alloys were fabricated using laser powder bed fusion (LPBF) starting from elementally blended Ni and Ti powders. Different melting strategies, including single and multiple melting, were studied in this work. Remelting improved the density and reduced cracking of the AM part. Microscopic observations, using a Scanning Electron Microscope (SEM) with a Backscattered Electron (BSE) detector, showed that the chemical homogeneity of the materials was enhanced by multiple remelting. Pure Ni and Ti were not found in any of the samples, proving that the applied melting strategies ensured good alloying of both powders. Regardless of the number of melting runs, X-ray diffraction (XRD) analysis showed the presence of NiTi (B2) and (B19′ ) phases, as well as NiTi2, Ni4Ti3 and Ni3Ti precipitates in all samples. The research demonstrated that, during the AM process, and depending on the melting strategy, 1.6–3.0 wt% of nickel evaporates from the material. It was demonstrated that the amount of evaporated nickel increased with the increasing number of melt cycles.peer-reviewe

Heat treatment of NiTi alloys fabricated using laser powder bed fusion (LPBF) from elementally blended powders

The use of elemental metallic powders and in situ alloying in additive manufacturing (AM) is of industrial relevance as it offers the required flexibility to tailor the batch powder composition. This solution has been applied to the AM manufacturing of nickel-titanium (NiTi) shape memory alloy components. In this work, we show that laser powder bed fusion (LPBF) can be used to create a Ni55.7Ti44.3 alloyed component, but that the chemical composition of the build has a large heterogeneity. To solve this problem three different annealing heat treatments were designed, and the resulting porosity, microstructural homogeneity, and phase formation was investigated. The heat treatments were found to improve the alloy’s chemical and phase homogeneity, but the brittle NiTi2 phase was found to be stabilized by the 0.54 wt.% of oxygen present in all fabricated samples. As a consequence, a Ni2Ti4O phase was formed and was confirmed by transmission electron microscopy (TEM) observation. This study showed that pore formation in in situ alloyed NiTi can be controlled via heat treatment. Moreover, we have shown that the two-step heat treatment is a promising method to homogenise the chemical and phase composition of in situ alloyed NiTi powder fabricated by LPBF.peer-reviewe

Laser and Electron Beam Additive Manufacturing Methods of Fabricating Titanium Bone Implants

Additive Manufacturing (AM) methods are generally used to produce an early sample or near net-shape elements based on three-dimensional geometrical modules. To date, publications on AM of metal implants have mainly focused on knee and hip replacements or bone scaffolds for tissue engineering. The direct fabrication of metallic implants can be achieved by methods, such as Selective Laser Melting (SLM) or Electron Beam Melting (EBM). This work compares the SLM and EBM methods used in the fabrication of titanium bone implants by analyzing the microstructure, mechanical properties and cytotoxicity. The SLM process was conducted in an environmental chamber using 0.4–0.6 vol % of oxygen to enhance the mechanical properties of a Ti-6Al-4V alloy. SLM processed material had high anisotropy of mechanical properties and superior UTS (1246–1421 MPa) when compared to the EBM (972–976 MPa) and the wrought material (933–942 MPa). The microstructure and phase composition depended on the used fabrication method. The AM methods caused the formation of long epitaxial grains of the prior β phase. The equilibrium phases (α + β) and non-equilibrium α’ martensite was obtained after EBM and SLM, respectively. Although it was found that the heat transfer that occurs during the layer by layer generation of the component caused aluminum content deviations, neither methods generated any cytotoxic effects. Furthermore, in contrast to SLM, the EBM fabricated material met the ASTMF136 standard for surgical implant applications

The Influence of Selective Laser Melting (SLM) Process Parameters on In-Vitro Cell Response

The use of laser 3D printers is very perspective in the fabrication of solid and porous implants made of various polymers, metals, and its alloys. The Selective Laser Melting (SLM) process, in which consolidated powders are fully melted on each layer, gives the possibility of fabrication personalized implants based on the Computer Aid Design (CAD) model. During SLM fabrication on a 3D printer, depending on the system applied, there is a possibility for setting the amount of energy density (J/mm3) transferred to the consolidated powders, thus controlling its porosity, contact angle and roughness. In this study, we have controlled energy density in a range 8–45 J/mm3 delivered to titanium powder by setting various levels of laser power (25–45 W), exposure time (20–80 µs) and distance between exposure points (20–60 µm). The growing energy density within studied range increased from 63 to 90% and decreased from 31 to 13 µm samples density and Ra parameter, respectively. The surface energy 55–466 mN/m was achieved with contact angles in range 72–128° and 53–105° for water and formamide, respectively. The human mesenchymal stem cells (hMSCs) adhesion after 4 h decreased with increasing energy density delivered during processing within each parameter group. The differences in cells proliferation were clearly seen after a 7-day incubation. We have observed that proliferation was decreasing with increasing density of energy delivered to the samples. This phenomenon was explained by chemical composition of oxide layers affecting surface energy and internal stresses. We have noticed that TiO2, which is the main oxide of raw titanium powder, disintegrated during selective laser melting process and oxygen was transferred into metallic titanium. The typical for 3D printed parts post-processing methods such as chemical polishing in hydrofluoric (HF) or hydrofluoric/nitric (HF/HNO3) acid solutions and thermal treatments were used to restore surface chemistry of raw powders and improve surface

Nanofunctionalization of Additively Manufactured Titanium Substrates for Surface-Enhanced Raman Spectroscopy Measurements

Powder bed fusion using a laser beam (PBF-LB) is a commonly used additive manufacturing (3D printing) process for the fabrication of various parts from pure metals and their alloys. This work shows for the first time the possibility of using PBF-LB technology for the production of 3D titanium substrates (Ti 3D) for surface-enhanced Raman scattering (SERS) measurements. Thanks to the specific development of the 3D titanium surface and its nanoscale modification by the formation of TiO2 nanotubes with a diameter of ~80 nm by the anodic oxidation process, very efficient SERS substrates were obtained after deposition of silver nanoparticles (0.02 mg/cm2, magnetron sputtering). The average SERS enhancement factor equal to 1.26 × 106 was determined for pyridine (0.05 M + 0.1 M KCl), as a model adsorbate. The estimated enhancement factor is comparable with the data in the literature, and the substrate produced in this way is characterized by the high stability and repeatability of SERS measurements. The combination of the use of a printed metal substrate with nanofunctionalization opens a new path in the design of SERS substrates for applications in analytical chemistry. Methods such as SEM scanning microscopy, photoelectron spectroscopy (XPS) and X-ray diffraction analysis (XRD) were used to determine the morphology, structure and chemical composition of the fabricated materials

Post Processing and Biological Evaluation of the Titanium Scaffolds for Bone Tissue Engineering

Nowadays, post-surgical or post-accidental bone loss can be substituted by custom-made scaffolds fabricated by additive manufacturing (AM) methods from metallic powders. However, the partially melted powder particles must be removed in a post-process chemical treatment. The aim of this study was to investigate the effect of the chemical polishing with various acid baths on novel scaffolds’ morphology, porosity and mechanical properties. In the first stage, Magics software (Materialise NV, Leuven, Belgium) was used to design a porous scaffolds with pore size equal to (A) 200 µm, (B) 500 µm and (C) 200 + 500 µm, and diamond cell structure. The scaffolds were fabricated from commercially pure titanium powder (CP Ti) using a SLM50 3D printing machine (Realizer GmbH, Borchen, Germany). The selective laser melting (SLM) process was optimized and the laser beam energy density in range of 91–151 J/mm3 was applied to receive 3D structures with fully dense struts. To remove not fully melted titanium particles the scaffolds were chemically polished using various HF and HF-HNO3 acid solutions. Based on scaffolds mass loss and scanning electron (SEM) observations, baths which provided most uniform surface cleaning were proposed for each porosity. The pore and strut size after chemical treatments was calculated based on the micro-computed tomography (µ-CT) and SEM images. The mechanical tests showed that the treated scaffolds had Young’s modulus close to that of compact bone. Additionally, the effect of pore size of chemically polished scaffolds on cell retention, proliferation and differentiation was studied using human mesenchymal stem cells. Small pores yielded higher cell retention within the scaffolds, which then affected their growth. This shows that in vitro cell performance can be controlled to certain extent by varying pore sizes

The Effect of Microstructural Defects on High-Cycle Fatigue of Ti Grade 2 Manufactured by PBF-LB and Hydrostatic Extrusion

The aim of this study was to show the effect of manufacturing defects in a commercially pure Ti Grade 2 produced by a laser beam powder bed fusion (PBF-LB) process on its high-cycle fatigue life. For this purpose, the high-cycle fatigue performance of PBF-LB Ti Grade 2 was compared to its ultrafine-grained (UFG) counterpart processed by hydrostatic extrusion exhibiting a similar mechanical properties under static tensile. The yield strength of the PBF-LB and UFG Ti Grade 2 was 740 and 783 MPa, respectively. The PBF-LB Ti Grade 2 consisted of a typical columnar of prior β grains with an acicular martensite α’ microstructure, while UFG Ti Grade 2 was mainly composed of fine, equiaxed α phase grains/subgrains with a size of 50–150 nm. A residual porosity of 0.21% was observed in the PBF-LB Ti Grade 2 by X-ray computed tomography, and, despite similar yield strength, a significantly higher endurance fatigue limit was noticed for UFG Ti Grade 2 (420 MPa) compared to PBF-LB Ti Grade 2 (330 MPa). Fatigue striation analysis showed that the fatigue crack propagation rate was not affected by manufacturing technology. In turn, the high-cycle fatigue life was drastically reduced as the size of manufacturing defects (such as pores or lack of fusion zones) increased