Micromechanical characterization of prismless enamel in the tuatara, Sphenodon punctatus.

Dental enamel - a naturally occurring biocomposite of mineral and protein - has evolved from a simple prismless to an advanced prismatic structure over millions of years. Exploring the mechanical function of its structural features with differing characteristics is of great importance for evolutionary developmental studies as well as for material scientists seeking to model the mechanical performance of biological materials. In this study, mechanical properties of prismless tuatara Sphenodon punctatus enamel were characterized. Using micro-cantilever bending samples the fracture strength and elastic modulus were found to be 640 ± 87 MPa and 42 ± 6 GPa, respectively in the orientation parallel to the crystallite long axis, which decreased in the orthogonal direction. The intrinsic fracture toughness of tuatara enamel ranged from 0.21 MPa m(1/2) and 0.32 MPa m(1/2). These values correspond to the lower limit of the range of values observed in prismatic enamel at the hierarchical level 1.

Hierarchical flexural strength of enamel: transition from brittle to damage-tolerant behaviour.

Hard, biological materials are generally hierarchically structured from the nano- to the macro-scale in a somewhat self-similar manner consisting of mineral units surrounded by a soft protein shell. Considerable efforts are underway to mimic such materials because of their structurally optimized mechanical functionality of being hard and stiff as well as damage-tolerant. However, it is unclear how different hierarchical levels interact to achieve this performance. In this study, we consider dental enamel as a representative, biological hierarchical structure and determine its flexural strength and elastic modulus at three levels of hierarchy using focused ion beam (FIB) prepared cantilevers of micrometre size. The results are compared and analysed using a theoretical model proposed by Jäger and Fratzl and developed by Gao and co-workers. Both properties decrease with increasing hierarchical dimension along with a switch in mechanical behaviour from linear-elastic to elastic-inelastic. We found Gao's model matched the results very well.

On the mechanical properties of hierarchically structured biological materials.

Many biological materials are hierarchically structured which means that they are designed from the nano- to the macro-scale in a sometimes self-similar way. There are lots of papers published including very detailed descriptions of these structures at all length scales--however, investigations of mechanical properties are most often focused on either nano-indentation or bulk mechanical testing characterizing properties at the smallest or largest size scale. Interestingly, there are hardly any investigations that systematically interconnect mechanical properties of different length scales. Nevertheless there are often conclusions drawn like the one that "biological materials exhibit their excellent mechanical properties due to their hierarchical structuring". Thus, we think there is a gap and discrepancy between the detection and description of biological structures and the correlated determination and interpretation of their mechanical properties. Hence, in this paper we order hierarchically structured biological materials with high mineral content according to their hierarchical levels and attribute measured mechanical properties to them. This offers the possibility to gain insight into the mechanical properties on different hierarchical levels even though the entire biological materials were tested. On the other hand we use data of one material, namely enamel, where mechanical properties were measured on every length scale. This kind of data analysis allows to show how a theoretical model developed by Huajian Gao and co-workers can be used to get closer insights into experimental data of hierarchically structured materials.

Mixed-mode stress intensity factors for kink cracks with finite kink length loaded in tension and bending: application to dentin and enamel.

Fracture toughness resistance curves describe a material's resistance against crack propagation. These curves are often used to characterize biomaterials like bone, nacre or dentin as these materials commonly exhibit a pronounced increase in fracture toughness with crack extension due to co-acting mechanisms such as crack bridging, crack deflection and microcracking. The knowledge of appropriate stress intensity factors which depend on the sample and crack geometry is essential for determining these curves. For the dental biomaterials enamel and dentin it was observed that, under bending and tensile loading, crack propagation occurs under certain constant angles to the initial notch direction during testing procedures used for fracture resistance curve determination. For this special crack geometry (a kink crack of finite length in a finite body) appropriate geometric function solutions are missing. Hence, we present in this study new mixed-mode stress intensity factors for kink cracks with finite kink length within samples of finite dimensions for two loading cases (tension and bending) which were derived from a combination of mixed-mode stress intensity factors of kink cracks with infinitely small kinks and of slant cracks. These results were further applied to determine the fracture resistance curves of enamel and dentin by testing single edge notched bending (SENB) specimens. It was found that kink cracks with finite kink length exhibit identical stress fields to slant cracks as soon as the kink length exceeds 0.15 times the initial straight crack or notch length. The use of stress intensity factor solutions for infinitely small kink cracks for the determination of dentin fracture resistance curves (as was done by other researchers) leads to an overestimation of dentin's fracture resistance of up to 30%.

Crack arrest within teeth at the dentinoenamel junction caused by elastic modulus mismatch.

Enamel and dentin compose the crowns of human teeth. They are joined at the dentinoenamel junction (DEJ) which is a very strong and well-bonded interface unlikely to fail within healthy teeth despite the formation of multiple cracks within enamel during a lifetime of exposure to masticatory forces. These cracks commonly are arrested when reaching the DEJ. The phenomenon of crack arrest at the DEJ is described in many publications but there is little consensus on the underlying cause and mechanism. Explanations range from the DEJ having a larger toughness than both enamel and dentin up to the assumption that not the DEJ itself causes crack arrest but the so-called mantle dentin, a thin material layer close to the DEJ that is somewhat softer than the bulk dentin. In this study we conducted 3-point bending experiments with bending bars consisting of the DEJ and surrounding enamel and dentin to investigate crack propagation and arrest within the DEJ region. Calculated stress intensities around crack tips were found to be highly influenced by the elastic modulus mismatch between enamel and dentin and hence, the phenomenon of crack arrest at the DEJ could be explained accordingly via this elastic modulus mismatch.

The fracture behaviour of dental enamel.

Enamel is the hardest tissue in the human body covering the crowns of teeth. Whereas the underlying dental material dentin is very well characterized in terms of mechanical and fracture properties, available data for enamel are quite limited and are apart from the most recent investigation mainly based on indentation studies. Within the current study, stable crack-growth experiments in bovine enamel have been performed, to measure fracture resistance curves for enamel. Single edge notched bending specimens (SENB) prepared out of bovine incisors were tested in 3-point bending and subsequently analysed using optical and environmental scanning electron microscopy. Cracks propagated primarily within the protein-rich rod sheaths and crack propagation occurred under an inclined angle to initial notch direction not only due to enamel rod and hydroxyapatite crystallite orientation but potentially also due to protein shearing. Determined mode I fracture resistance curves ranged from 0.8-1.5 MPa*m(1/2) at the beginning of crack propagation up to 4.4 MPa*m(1/2) at 500 microm crack extension; corresponding mode II values ranged from 0.3 to 1.5 MPa*m(1/2).