Claudia Fleck

Toughening and functionalization of bioactive ceramic and glass bone scaffolds by biopolymer coatings and infiltration: a review of the last 5 years

Inorganic scaffolds with high interconnected porosity based on bioactive glasses and ceramics are prime candidates for applications in bone tissue engineering. These materials however exhibit relatively low fracture strength and high brittleness. A simple and effective approach to improve the toughness is to combine the basic scaffold structure with polymer coatings or through the formation of interpenetrating polymer-bioactive ceramic microstructures. The polymeric phase can additionally serve as a carrier for growth factors and therapeutic drugs, thus adding biological functionalities. The present paper reviews the state-of-the art in the field of polymer coated and infiltrated bioactive inorganic scaffolds. Based on the notable combination of bioactivity, improved mechanical properties and drug or growth factor delivery capability, this scaffold type is a candidate for bone and osteochondral regeneration strategies. Remaining challenges for the improvement of the materials are discussed and opportunities to broaden the application potential of this scaffold type are also highlighted.

Compressive Residual Strains in Mineral Nanoparticles as a Possible Origin of Enhanced Crack Resistance in Human Tooth Dentin

The tough bulk of dentin in teeth supports enamel, creating cutting and grinding biostructures with superior failure resistance that is not fully understood. Synchrotron-based diffraction methods, utilizing micro- and nanofocused X-ray beams, reveal that the nm-sized mineral particles aligned with collagen are precompressed and that the residual strains vanish upon mild annealing. We show the link between the mineral nanoparticles and known damage propagation trajectories in dentin, suggesting a previously overlooked compression-mediated toughening mechanism.

Characterizing the transformation near indents and cracks in clinically used dental yttria-stabilized zirconium oxide constructs

OBJECTIVES Tetragonal zirconia polycrystal (TZP) materials are widely used for full ceramic partial dentures, even though their mechanical properties might change during service. A key property for the durability of the constructs is thought to be an inhibition of crack propagation by phase transformation toughening. Because dental prosthesis are ground and polished for adjustment purposes, it is important to understand the effects of mechanical surface treatments, on localized transformation and around the propagating cracks. METHODS Sintered samples of commercially available 3 mol-% Yittria-doped TZP were ground and polished and the surface structure and phase composition were compared with those of re-transformed annealed samples. Microindentation was used to induce cracks and nanoindentation was performed to determine the local variety of hardness and indentation modulus, coupled with XRD and SEM investigations. RESULTS Y-TZP polished surfaces exhibited 9% monoclinic phase content and have reduced hardness and indentation modulus amounting 16.3 GPa and 210.6 GPa, respectively. Y-TZP re-transformed annealed sample revealed 19.4 GPa and 242.3 GPa, respectively. A localized reduction of the stiffness around the crack tips on the annealed surface reveals an irregular arrangement of t-m-transformed grains. Electron micrographs show more damage on the transformed surface following microindentation than on indented annealed surfaces. SIGNIFICANCE Y-TZP prostheses are adapted and roughened by clinicians prior to bonding to teeth. Annealing recovers properties and microstructure that is changed by the adaptation of the outer layer. This might be important to ensure long-term toughening functionality of the dentures and optimal comfort for the patients.

Biomimetic cellular metals—using hierarchical structuring for energy absorption

Fruit walls as well as nut and seed shells typically perform a multitude of functions. One of the biologically most important functions consists in the direct or indirect protection of the seeds from mechanical damage or other negative environmental influences. This qualifies such biological structures as role models for the development of new materials and components that protect commodities and/or persons from damage caused for example by impacts due to rough handling or crashes. We were able to show how the mechanical properties of metal foam based components can be improved by altering their structure on various hierarchical levels inspired by features and principles important for the impact and/or puncture resistance of the biological role models, rather than by tuning the properties of the bulk material. For this various investigation methods have been established which combine mechanical testing with different imaging methods, as well as with in situ and ex situ mechanical testing methods. Different structural hierarchies especially important for the mechanical deformation and failure behaviour of the biological role models, pomelo fruit (Citrus maxima) and Macadamia integrifolia, were identified. They were abstracted and transferred into corresponding structural principles and thus hierarchically structured bio-inspired metal foams have been designed. A production route for metal based bio-inspired structures by investment casting was successfully established. This allows the production of complex and reliable structures, by implementing and combining different hierarchical structural elements found in the biological concept generators, such as strut design and integration of fibres, as well as by minimising casting defects. To evaluate the structural effects, similar investigation methods and mechanical tests were applied to both the biological role models and the metallic foams. As a result an even deeper quantitative understanding of the form-structure-function relationship of the biological concept generators as well as the bio-inspired metal foams was achieved, on deeper hierarchical levels and overarching different levels.

Tetragonal and cubic zirconia multilayered ceramic constructs created by EPD.

The interest in electrophoretic deposition (EPD) for nanomaterials and ceramics production has widely increased due to the versatility of this technique to effectively combine different materials in unique shapes and structures. We successfully established an EPD layering process with submicrometer sized powders of Y-TZP with different mol percentages of yttrium oxide (3 and 8%) and produced multilayers of alternating tetragonal and cubic phases with a clearly defined interface. The rationale behind the design of these multilayer constructs was to optimize the properties of the final ceramic by combining the high mechanical toughness of the tetragonal phase of zirconia together with the high ionic conductivity of its cubic phase. In this work, a preliminary study of the mechanical properties of these constructs proved the good mechanical integrity of the multilayered constructs obtained as well as crack deflection in the interface between tetragonal and cubic zirconia layers.

Fruit walls and nut shells as an inspiration for the design of bio-inspired impact resistant hierarchically structured materials

Until today the structuring of different types of fruit walls has been used only as an inspiration for packaging when seen from a biomimetic perspective. However, by a detailed investigation of the Macadamia nut with its tough testa, Citrus maxima, possessing a large spongy mesocarp and Cocos nucifera, having a combination of a fi brous mesocarp and a tough endocarp, it becomes evident that those structures also provide excellent biological role models for impactand puncture-resistant materials. Both Citrus maxima and Cocos nucifera are relatively heavy, lack any aerodynamic adaptation and share the same challenge of having to withstand the impact from heights of >10 m. Conducting high-speed camera-controlled free fall experiments of Citrus maxima from 6 m height, we could demonstrate a deceleration of the fruits of 3100 m/s2, which corresponds to 316 g, without any visible damage of the fruit. An analysis using cyclic quasi-static compression tests of the pericarp of Citrus maxima revealed that the material behaves constant in good approximation after the fi rst loading cycle. During the fi rst cycle, almost 75% of the energy is dissipated. The pericarp of Citrus maxima is highly visco-elastic, which causes the samples within 1 min to recover 30% of their initial deformation caused by loading to 40% strain. The mesocarp of Citrus maxima is best described as an open-pore foam with a gradual increase in the pore size. Understanding the principles of as to how combining the structure and material in biological constructions yields a fully functional protection layer will allow us to construct new lightweight bio-inspired materials of high impact and puncture resistance with a combination of high energy dissipation, benign failure and almost complete recovery from large deformations.

In situ compressibility of carbonated hydroxyapatite in tooth dentine measured under hydrostatic pressure by high energy X-ray diffraction

Tooth dentine and other bone-like materials contain carbonated hydroxyapatite nanoparticles within a network of collagen fibrils. It is widely assumed that the elastic properties of biogenic hydroxyapatites are identical to those of geological apatite. By applying hydrostatic pressure and by in situ measurements of the a- and c- lattice parameters using high energy X-ray diffraction, we characterize the anisotropic deformability of the mineral in the crowns and roots of teeth. The collected data allowed us to calculate the bulk modulus and to derive precise estimates of Young׳s moduli and Poisson׳s ratios of the biogenic mineral particles. The results show that the dentine apatite particles are about 20% less stiff than geological and synthetic apatites and that the mineral has an average bulk modulus K=82.7 GPa. A 5% anisotropy is observed in the derived values of Young׳s moduli, with E11≈91 GPa and E33≈96 GPa, indicating that the nanoparticles are only slightly stiffer along their long axis. Poisson׳s ratio spans ν≈0.30-0.35, as expected. Our findings suggest that the carbonated nanoparticles of biogenic apatite are significantly softer than previously thought and that their elastic properties can be considered to be nearly isotropic.

Structure-Function Relationships in Macadamia integrifolia Seed Coats – Fundamentals of the Hierarchical Microstructure

The shells/coats of nuts and seeds are often very hard to crack. This is particularly the case with Macadamia seed coats, known to exhibit astoundingly high strength and toughness. We performed an extensive materials science characterization of the complex hierarchical structure of these coats, using light and scanning electron microscopy in 2D as well as microCT for 3D characterization. We differentiate nine hierarchical levels that characterize the structure ranging from the whole fruit on the macroscopic scale down to the molecular scale. From a biological viewpoint, understanding the hierarchical structure may elucidate why it is advantageous for these seed coats to be so difficult to break. From an engineering viewpoint, microstructure characterization is important for identifying features that contribute to the high strength and cracking resistance of these objects. This is essential for revealing the underlying structure-function-relationships. Such information will help us develop engineering materials and lightweight-structures with improved fracture and puncture resistance.

Importance of the variable periodontal ligament geometry for whole tooth mechanical function: A validated numerical study

When mammalian teeth breakdown food, several juxtaposed dental tissues work mechanically together, while balancing requirements of food comminution and avoiding damage to the oral tissues. One important way to achieve this is by channeling mastication forces into the surrounding jaw bone through a thin and compliant soft tissue, the periodontal ligament (PDL). As a result, during a typical chewing stroke, each tooth moves quite substantially in its anchor-site. Here we report a series of experiments, where we study the reaction of three-rooted teeth to a single chewing event by finite element (FE) modelling. The nonlinear behaviour of the PDL is simulated by a hyperelastic material model and the in silico results are validated by our own in vitro experiments. We examine the displacement response of the complete tooth-PDL-bone complex to increasing chewing loads. We observe that small spatially-varying geometric adjustments to the thickness of the PDL lead to strong changes in observed tooth reaction movement, as well as PDL strain and bone stress. When reproducing the regionally varying thickness of the PDL observed in vivo, FE simulations reveal subtle but significant tooth motion that leads to an even distribution of the stresses in the jaw bone, and to lower strains in the PDL. Our in silico experiments also reproduce the results of experiments performed by others on different animal models and are therefore useful for overcoming the difficulties of obtaining tooth-PDL-bone loading estimates in vivo. This data thus enhances our understanding of the role the variable PDL geometry plays in the tooth-PDL-bone complex during mastication.

Cyclic deformation behaviour of (α + β) titanium alloys under complex mechanical and physiological loading conditions: Dedicated to Professor Dr. Haël Mughrabi on the occasion of his 65th birthday

Abstract In the present investigation, the cyclic deformation behaviour of TiAl6V4 and TiAl6Nb7 was characterized in constant-amplitude and load increase tests in laboratory air and quasi-physiolog...