Karel Lietaert

Additively manufactured metallic porous biomaterials based on minimal surfaces : A unique combination of topological, mechanical, and mass transport properties

Porous biomaterials that simultaneously mimic the topological, mechanical, and mass transport properties of bone are in great demand but are rarely found in the literature. In this study, we rationally designed and additively manufactured (AM) porous metallic biomaterials based on four different types of triply periodic minimal surfaces (TPMS) that mimic the properties of bone to an unprecedented level of multi-physics detail. Sixteen different types of porous biomaterials were rationally designed and fabricated using selective laser melting (SLM) from a titanium alloy (Ti-6Al-4V). The topology, quasi-static mechanical properties, fatigue resistance, and permeability of the developed biomaterials were then characterized. In terms of topology, the biomaterials resembled the morphological properties of trabecular bone including mean surface curvatures close to zero. The biomaterials showed a favorable but rare combination of relatively low elastic properties in the range of those observed for trabecular bone and high yield strengths exceeding those reported for cortical bone. This combination allows for simultaneously avoiding stress shielding, while providing ample mechanical support for bone tissue regeneration and osseointegration. Furthermore, as opposed to other AM porous biomaterials developed to date for which the fatigue endurance limit has been found to be ≈20% of their yield (or plateau) stress, some of the biomaterials developed in the current study show extremely high fatigue resistance with endurance limits up to 60% of their yield stress. It was also found that the permeability values measured for the developed biomaterials were in the range of values reported for trabecular bone. In summary, the developed porous metallic biomaterials based on TPMS mimic the topological, mechanical, and physical properties of trabecular bone to a great degree. These properties make them potential candidates to be applied as parts of orthopedic implants and/or as bone-substituting biomaterials. STATEMENT OF SIGNIFICANCE Bone-substituting biomaterials aim to mimic bone properties. Although mimicking some of bone properties is feasible, biomaterials that could simultaneously mimic all or most of the relevant bone properties are rare. We used rational design and additive manufacturing to develop porous metallic biomaterials that exhibit an interesting combination of topological, mechanical, and mass transport properties. The topology of the developed biomaterials resembles that of trabecular bone including a mean curvature close to zero. Moreover, the developed biomaterials show an unusual combination of low elastic modulus to avoid stress shielding and high strength to provide mechanical support. The fatigue resistance of the developed biomaterials is also exceptionally high, while their permeability is in the range of values reported for bone.

Improving the fatigue performance of porous metallic biomaterials produced by Selective Laser Melting

This paper provides new insights into the fatigue properties of porous metallic biomaterials produced by additive manufacturing. Cylindrical porous samples with diamond unit cells were produced from Ti6Al4V powder using Selective Laser Melting (SLM). After measuring all morphological and quasi-static properties, compression-compression fatigue tests were performed to determine fatigue strength and to identify important fatigue influencing factors. In a next step, post-SLM treatments were used to improve the fatigue life of these biomaterials by changing the microstructure and by reducing stress concentrators and surface roughness. In particular, the influence of stress relieving, hot isostatic pressing and chemical etching was studied. Analytical and numerical techniques were developed to calculate the maximum local tensile stress in the struts as function of the strut diameter and load. With this method, the variability in the relative density between all samples was taken into account. The local stress in the struts was then used to quantify the exact influence of the applied post-SLM treatments on the fatigue life. A significant improvement of the fatigue life was achieved. Also, the post-SLM treatments, procedures and calculation methods can be applied to different types of porous metallic structures and hence this paper provides useful tools for improving fatigue performance of metallic biomaterials. STATEMENT OF SIGNIFICANCE Additive Manufacturing (AM) techniques such as Selective Laser Melting (SLM) are increasingly being used for producing customized porous metallic biomaterials. These biomaterials are regularly used for biomedical implants and hence a long lifetime is required. In this paper, a set of post-built surface and heat treatments is presented that can be used to significantly improve the fatigue life of porous SLM-Ti6Al4V samples. In addition, a novel and efficient analytical local stress method was developed to accurately quantify the influence of the post-built treatments on the fatigue life. Also numerical simulation techniques were used for validation. The developed methods and techniques can be applied to other types of porous biomaterials and hence provide new and useful tools for improving and predicting the fatigue life of porous biomaterials.

Antibacterial behavior of additively manufactured porous titanium with nanotubular surfaces releasing silver ions

Additive manufacturing (3D printing) has enabled fabrication of geometrically complex and fully interconnected porous biomaterials with huge surface areas that could be used for biofunctionalization to achieve multifunctional biomaterials. Covering the huge surface area of such porous titanium with nanotubes has been already shown to result in improved bone regeneration performance and implant fixation. In this study, we loaded TiO2 nanotubes with silver antimicrobial agents to equip them with an additional biofunctionality, i.e., antimicrobial behavior. An optimized anodizing protocol was used to create nanotubes on the entire surface area of direct metal printed porous titanium scaffolds. The nanotubes were then loaded by soaking them in three different concentrations (i.e., 0.02, 0.1, and 0.5 M) of AgNO3 solution. The antimicrobial behavior and cell viability of the developed biomaterials were assessed. As far as the early time points (i.e., up to 1 day) are concerned, the biomaterials were found to be extremely effective in preventing biofilm formation and decreasing the number of planktonic bacteria particularly for the middle and high concentrations of silver ions. Interestingly, nanotubes not loaded with antimicrobial agents also showed significantly smaller numbers of adherent bacteria at day 1, which may be attributed to the bactericidal effect of high aspect ratio nanotopographies. The specimens with the highest concentrations of antimicrobial agents adversely affected cell viability at day 1, but this effect is expected to decrease or disappear in the following days as the rate of release of silver ions was observed to markedly decrease within the next few days. The antimicrobial effects of the biomaterials, particularly the ones with the middle and high concentrations of antimicrobial agents, continued until 2 weeks. The potency of the developed biomaterials in decreasing the number of planktonic bacteria and hindering the formation of biofilms make them promising candidates for combating peri-operative implant-associated infections.

Fatigue performance of additively manufactured meta-biomaterials: The effects of topology and material type

Additive manufacturing (AM) techniques enable fabrication of bone-mimicking meta-biomaterials with unprecedented combinations of topological, mechanical, and mass transport properties. The mechanical performance of AM meta-biomaterials is a direct function of their topological design. It is, however, not clear to what extent the material type is important in determining the fatigue behavior of such biomaterials. We therefore aimed to determine the isolated and modulated effects of topological design and material type on the fatigue response of metallic meta-biomaterials fabricated with selective laser melting. Towards that end, we designed and additively manufactured Co-Cr meta-biomaterials with three types of repeating unit cells and three to four porosities per type of repeating unit cell. The AM meta-biomaterials were then mechanically tested to obtain their normalized S-N curves. The obtained S-N curves of Co-Cr meta-biomaterials were compared to those of meta-biomaterials with same topological designs but made from other materials, i.e. Ti-6Al-4V, tantalum, and pure titanium, available from our previous studies. We found the material type to be far more important than the topological design in determining the normalized fatigue strength of our AM metallic meta-biomaterials. This is the opposite of what we have found for the quasi-static mechanical properties of the same meta-biomaterials. The effects of material type, manufacturing imperfections, and topological design were different in the high and low cycle fatigue regions. That is likely because the cyclic response of meta-biomaterials depends not only on the static and fatigue strengths of the bulk material but also on other factors that may include strut roughness, distribution of the micro-pores created inside the struts during the AM process, and plasticity. STATEMENT OF SIGNIFICANCE Meta-biomaterials are a special class of metamaterials with unusual or unprecedented combinations of mechanical, physical (e.g. mass transport), and biological properties. Topologically complex and additively manufactured meta-biomaterials have been shown to improve bone regeneration and osseointegration. The mechanical properties of such biomaterials are directly related to their topological design and material type. However, previous studies of such biomaterials have largely neglected the effects of material type, instead focusing on topological design. We show here that neglecting the effects of material type is unjustified. We studied the isolated and combined effects of topological design and material type on the normalized S-N curves of metallic bone-mimicking biomaterials and found them to be more strongly dependent on the material type than topological design.

CoCr F75 scaffolds produced by additive manufacturing: Influence of chemical etching on powder removal and mechanical performance

Additive manufacturing techniques such as Selective Laser Melting (SLM) allow carefully controlled production of complex porous structures such as scaffolds. These advanced structures can offer many interesting advantages over conventionally produced products in terms of biological response and patient specific design. The surface finish of AM parts is often poor because of the layer wise nature of the process and adhering particles. Loosening of these particles after implantation should be avoided, as this could put the patients health at risk. In this study the use of hydrochloric acid and hydrogen peroxide mixtures for surface treatment of cobalt-chromium F75 scaffolds produced by SLM is investigated. A 27% HCl and 8% H2O2 etchant proved effective in removing adhering particles while retaining the quasi-static and fatigue performance of the scaffolds.

Effects of applied stress ratio on the fatigue behavior of additively manufactured porous biomaterials under compressive loading

Additively manufactured (AM) porous metallic biomaterials are considered promising candidates for bone substitution. In particular, AM porous titanium can be designed to exhibit mechanical properties similar to bone. There is some experimental data available in the literature regarding the fatigue behavior of AM porous titanium, but the effect of stress ratio on the fatigue behavior of those materials has not been studied before. In this paper, we study the effect of applied stress ratio on the compression-compression fatigue behavior of selective laser melted porous titanium (Ti-6Al-4V) based on the diamond unit cell. The porous titanium biomaterial is treated as a meta-material in the context of this work, meaning that R-ratios are calculated based on the applied stresses acting on a homogenized volume. After morphological characterization using micro computed tomography and quasi-static mechanical testing, the porous structures were tested under cyclic loading using five different stress ratios, i.e. R = 0.1, 0.3, 0.5, 0.7 and 0.8, to determine their S-N curves. Feature tracking algorithms were used for full-field deformation measurements during the fatigue tests. It was observed that the S-N curves of the porous structures shift upwards as the stress ratio increases. The stress amplitude was the most important factor determining the fatigue life. Constant fatigue life diagrams were constructed and compared with similar diagrams for bulk Ti-6Al-4V. Contrary to the bulk material, there was limited dependency of the constant life diagrams to mean stress. The notches present in the AM biomaterials were the sites of crack initiation. This observation and other evidence suggest that the notches created by the AM process cause the insensitivity of the fatigue life diagrams to mean stress. Feature tracking algorithms visualized the deformation during fatigue tests and demonstrated the root cause of inclined (45°) planes of specimen failure. In conclusion, the R-ratio behavior of AM porous biomaterials is both quantitatively and qualitatively different from that of bulk materials.

Rationally designed meta-implants: a combination of auxetic and conventional meta-biomaterials

Rationally designed meta-biomaterials present unprecedented combinations of mechanical, mass transport, and biological properties favorable for tissue regeneration. Here we introduce hybrid meta-biomaterials with rationally-distributed values of negative (auxetic) and positive Poissons ratios, and use them to design meta-implants that unlike conventional implants do not retract from the bone under biomechanical loading. We rationally design and additively manufacture six different types of meta-biomaterials (three auxetic and three conventional), which then serve as the parent materials to six hybrid meta-biomaterials (with or without transitional regions). Both single and hybrid meta-biomaterials are mechanically tested to reveal their full-field strain distribution by digital image correlation. The best-performing hybrid meta-biomaterials are then selected for the design of meta-implants (hip stems), which are tested under simulated-implantation conditions. Full-field strain measurements clearly show that, under biomechanical loading, hybrid meta-implants press onto the bone on both the medial and lateral sides, thereby improving implant–bone contact and potentially implant longevity.

Isolated and modulated effects of topology and material type on the mechanical properties of additively manufactured porous biomaterials

In this study, we tried to quantify the isolated and modulated effects of topological design and material type on the mechanical properties of AM porous biomaterials. Towards this aim, we assembled a large dataset comprising the mechanical properties of AM porous biomaterials with different topological designs (i.e. different unit cell types and relative densities) and material types. Porous structures were additively manufactured from Co-Cr using a selective laser melting (SLM) machine and tested under quasi-static compression. The normalized mechanical properties obtained from those structures were compared with mechanical properties available from our previous studies for porous structures made from Ti-6Al-4V and pure titanium as well as with analytical solutions. The normalized values of elastic modulus and yield stress were found to be relatively close to each other as well as in agreement with analytical solutions regardless of material type. However, the material type was found to systematically affect the mechanical properties of AM porous biomaterials in general and the post-elastic/post-yield range (plateau stress and energy absorption capacity) in particular. To put this in perspective, topological design could cause up to 10-fold difference in the mechanical properties of AM porous biomaterials while up to 2-fold difference was observed as a consequence of changing the material type.

Simultaneous Delivery of Multiple Antibacterial Agents from Additively Manufactured Porous Biomaterials to Fully Eradicate Planktonic and Adherent Staphylococcus aureus

Implant-associated infections are notoriously difficult to treat and may even result in amputation and death. The first few days after surgery are the most critical time to prevent those infections, preferably through full eradication of the micro-organisms entering the body perioperatively. That is particularly important for patients with a compromised immune system such as orthopedic oncology patients, as they are at higher risk for infection and complications. Full eradication of bacteria is, especially in a biofilm, extremely challenging due to the toxicity barrier that prevents delivery of high doses of antibacterial agents. This study aimed to use the potential synergistic effects of multiple antibacterial agents to prevent the use of toxic levels of these agents and achieve full eradication of planktonic and adherent bacteria. Silver ions and vancomycin were therefore simultaneously delivered from additively manufactured highly porous titanium implants with an extremely high surface area incorporating a bactericidal coating made from chitosan and gelatin applied by electrophoretic deposition (EPD). The presence of the chitosan/gelatin (Ch+Gel) coating, Ag, and vancomycin (Vanco) was confirmed by X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR). The release of vancomycin and silver ions continued for at least 21 days as measured by inductively coupled plasma (ICP) and UV-spectroscopy. Antibacterial behavior against Staphylococcus aureus, both planktonic and in biofilm, was evaluated for up to 21 days. The Ch+Gel coating showed some bactericidal behavior on its own, while the loaded hydrogels (Ch+Gel+Ag and Ch+Gel+Vanco) achieved full eradication of both planktonic and adherent bacteria without causing significant levels of toxicity. Combining silver and vancomycin improved the release profiles of both agents and revealed a synergistic behavior that further increased the bactericidal effects.

Mathematical modelling of the degradation behaviour of biodegradable metals

A mathematical model for the biodegradation of magnesium is developed in this study to inspect the corrosion behaviour of biodegradable implants. The aim of this study was to provide a suitable framework for the assessment of the corrosion rate of magnesium which includes the process of formation/dissolution of the protective film. The model is intended to aid the design of implants with suitable geometries. The level-set method is used to follow the changing geometry of the implants during the corrosion process. A system of partial differential equations is formulated based on the physical and chemical processes that occur at the implant-medium boundary in order to simulate the effect of the formation of a protective film on the degradation rate. The experimental data from the literature on the corrosion of a high-purity magnesium sample immersed in simulated body fluid is used to calibrate the model. The model is then used to predict the degradation behaviour of a porous orthopaedic implant. The model successfully reproduces the precipitation of the corrosion products on the magnesium surface and the effect on the degradation rate. It can be used to simulate the implant degradation and the formation of the corrosion products on the surface of biodegradable magnesium implants with complex geometries.