Fracture Toughness Properties of Three Different Biomaterials Measured by Nanoindentation

The fracture toughness of hard biomaterials, such as nacre, bovine hoof wall and beetle cuticle, is associated with fibrous or lamellar structures that deflect or stop growing cracks. Their hardness and reduced modulus were measured by using a nanoindenter in this paper. Micro/nanoscale cracks were generated by nanoindentation using a Berkovich tip. Nanoindentation of nacre and bovine hoof wall resulted in pile-up around the indent. It was found that the fracture toughness （Kc） of bovine hoof wall is the maximum, the second is nacre, and the elytra cuticle of dung beetle is the least one.     

Nanoscale structure and mechanical behavior of growth lines in shell of abalone Haliotis gigantea

In the natural world, bottom-up hierarchical construction of complex structures results in materials with remarkable properties. A well known example is the nacre of mollusk shells, commonly called "mother of pearl", whose excellent strength and toughness has been the subject of research for many decades. A significant discovery has been the presence of periodic layers called "growth lines". These are thin distinct layers within the bulk of the shell which form periodically, with their structure affected by environmental changes. Studies of their formation and behavior offer valuable insight into the architecture of seashells. In this work, the structure and mechanical behavior of growth lines in shells of abalone Haliotis gigantea were investigated using electron microscopy and nanoindentation. Growth lines form directly out of nacre into layers of blocks and irregular particles. In comparison to nacre, they have basic structures, form rapidly, and are harder, which suggest that they serve a protective role during lifecycle transitions. This exemplifies how natural structures are able to closely control growth architecture in order to form different structures for different functions, all from the same base materials.     

On the fracture mechanisms of nacre: Effects of structural orientation

The nacre of mollusk shells is distinguished by an exceptional mechanical efficiency which is derived essentially from its lamellar structure and frequently acts as a source of inspiration for the development of biomimetic materials. The structure and mechanical properties of nacre have been intensively investigated with a special focus on its toughening strategies; nevertheless, the fracture mechanisms, more specifically the critical stress/strain conditions for the failure of nacre, and the effects of structural orientation and hydration state remain largely unexplored. Here uniaxial compression tests were performed on nacre of both dry and hydrated states with different off-axis angles, i.e., the inclination of loading axis with respect to the lamellar structure, ranging from 0° to 90°. The mechanical properties and fracture characteristics of nacre and their dependences on the structural orientation and hydration state were elucidated in terms of mechanics behind failure. Quantitative relationships were established between the mechanical properties and off-axis angle based on different failure criteria. The competition between the fracture modes of fragmentation and shearing was quantified by comparing their respective driving force and resistance on the interfacial plane. This study may aid the understanding on the mechanical behavior of nacre and nacre-inspired synthetic materials and promote a better replication of the underlying design principles of nacre in man-made systems.     

Unlocalized crack initiation and propagation in staggered biomaterials

Many types of tissues in living organisms exhibit a combination of different properties to fulfil their mechanical functions in complex environments. Nacre with more than 90% brittle and hard phase and a little protein matrix, exhibits high strength and toughness, which is difficult to achieve in artificial materials. Researchers have shown that the toughness of nacre is related to the cracking process. Most of them, however, assume an obvious pre-existing crack on the model and the initiation of the microscopical pre-existing crack is not considered yet. Based on fracture mechanics with the cohesive zone model, we reveal the mechanism of the crack initiation and propagation pattern in staggered biomaterials without any pre-existing crack. The simulation result shows that there are two crack propagation modes: localized mode and unlocalized mode. A crack initiates and propagates in a small area in the localized mode, while cracks initiate at different points and propagate in various paths in the unlocalized mode. The crack initiation mechanism from the intrinsic properties of the material is clarified using energy based stability analysis. The result shows that the shear interfacial mechanism significantly delays the crack initiation.     

Br-rich tips of calcified crab claws are less hard but more fracture resistant: A comparison of mineralized and heavy-element biological materials

We find that the spoon-like tips of the chelipeds (large claws) of the crab Pachygrapsus crassipes differ from the rest of the claw in that they are not calcified, but instead contain about 1% bromine—thus they represent a new example of a class of structural biological materials that contain heavy elements such as Zn, Mn, Fe, Cu, and Br bound in an organic matrix. X-ray absorption spectroscopy data suggest that the bromine is bound to phenyl rings, possibly in tyrosine. We measure a broad array of mechanical properties of a heavy-element biological material for the first time (abrasion resistance, coefficient of kinetic friction, energy of fracture, hardness, modulus of elasticity and dynamic mechanical properties), and we make a direct comparison with a mineralized tissue. Our results suggest that the greatest advantage of bromine-rich cuticle over calcified cuticle is resistance to fracture (the energy of fracture is about an order of magnitude greater than for calcified cuticle). The greatest advantage relative to unenriched cuticle, represented by ant mandible cuticle, is a factor of about 1.5 greater hardness and modulus of elasticity. The spoon-like tips gain additional fracture resistance from the orientation of the constituent laminae and from the viscoelasticity of the material. We suggest that fracture resistance is of greater importance in smaller organisms, and we speculate that one function of heavy elements in structural biological materials is to reduce molecular resonant frequencies and thereby increase absorption of energy from impacts.     

Influence of loading condition and anatomical location on human cortical bone linear micro-cracks

Human cortical bone fracture toughness depends on the anatomical locations under quasi-static loading. Recent results also showed that under fall-like loading, cortical bone fracture toughness is similar at different anatomical locations in the same donor. While cortical bone toughening mechanisms are known to be dependent on the tissue architecture under quasi-static loading, the fracture mechanisms during a fall are less studied. In the current study, the structural parameters of eight paired femoral diaphyses, femoral necks and radial diaphyses were mechanically tested under quasi-static and fall-like loading conditions (female donors, 70 ± 14 y.o., [50–91 y.o.]). Synchrotron radiation micro-CT imaging was used to quantify the amount of micro-cracks formed during loading. The volume fraction of these micro-cracks was significantly higher within the specimens loaded under a quasi-static condition than under a loading representative of a fall. Under fall-like loading, there was no difference in crack volume fraction between the different paired anatomical locations. This result shows that the micro-cracking toughening mechanism depends both on the anatomical location and on the loading condition.     

Instrumented Indentation Investigation on the Viscoelastic Properties of Porcine Cartilage

Articular cartilage lubricates the contact surfaces in human joints and provides a shock-absorbing effect which protects the joint under dynamic loading. However, this shock-absorbing effect is gradually reduced as the result of normal wear, tear and aging-related cartilage loss. Thus, with the increasing average human life expectancy, the issue of joint health has attracted significant interest in recent decades. In developing new materials for the repair or regeneration of damaged articular cartilage, it is essential that the difference in the mechanical properties of healthy and damaged cartilages is well-understood. In the present study, the hardness and Young＇s modulus of damaged and healthy porcine articular cartilage samples are evaluated via a quasi-static nanoindentation technique. A dynamic mechanical analysis method is then applied to determine the viscoelastic properties of the two samples. The results presented in this study provide a useful insight into the mechanical properties of articular cartilage at the mesoscale, and therefore fill an important gap in the literature.     

Adaptation to hard-object feeding in sea otters and hominins

The large, bunodont postcanine teeth in living sea otters (Enhydra lutris) have been likened to those of certain fossil hominins, particularly the ’robust’ australopiths (genus Paranthropus). We examine this evolutionary convergence by conducting fracture experiments on extracted molar teeth of sea otters and modern humans (Homo sapiens) to determine how load-bearing capacity relates to tooth morphology and enamel material properties. In situ optical microscopy and x-ray imaging during simulated occlusal loading reveal the nature of the fracture patterns. Explicit fracture relations are used to analyze the data and to extrapolate the results from humans to earlier hominins. It is shown that the molar teeth of sea otters have considerably thinner enamel than those of humans, making sea otter molars more susceptible to certain kinds of fractures. At the same time, the base diameter of sea otter first molars is larger, diminishing the fracture susceptibility in a compensatory manner. We also conduct nanoindentation tests to map out elastic modulus and hardness of sea otter and human molars through a section thickness, and microindentation tests to measure toughness. We find that while sea otter enamel is just as stiff elastically as human enamel, it is a little softer and tougher. The role of these material factors in the capacity of dentition to resist fracture and deformation is considered. From such comparisons, we argue that early hominin species like Paranthropus most likely consumed hard food objects with substantially higher biting forces than those exerted by modern humans.     

Gastropod nacre: structure, properties and growth--biological, chemical and physical basics

The biogenic polymer/mineral composite nacre is a non-brittle biological ceramic, which self-organizes in aqueous environment and under ambient conditions. It is therefore an important model for new sustainable materials. Its highly controlled structural organization of mineral and organic components at all scales down to the nano- and molecular scales is guided by organic molecules. These molecules then get incorporated into the material to be responsible for properties like fracture mechanics, beauty and corrosion resistance. We report here on structure, properties and growth of columnar (gastropod) nacre with emphasis on the genus Haliotis in contrast to sheet nacre of many bivalves.     

In vivo analysis of fracture toughness of thyroid gland tumors

Background

Human solid tumors that are hard or firm on physical palpation are likely to be cancerous, a clinical maxim that has been successfully applied to cancer screening programs, such as breast self-examination. However, the biological relevance or prognostic significance of tumor hardness remains poorly understood. Here we present a fracture mechanics based in vivo approach for characterizing the fracture toughness of biological tissue of human thyroid gland tumors.

Methods

In a prospective study, 609 solid thyroid gland tumors were percutaneously probed using standard 25 gauge fine needles, their tissue toughness ranked on the basis of the nature and strength of the haptic force feedback cues, and subjected to standard fine needle biopsy. The tumors' toughness rankings and final cytological diagnoses were combined and analyzed. The interpreting cytopathologist was blinded to the tumors' toughness rankings.

Results

Our data showed that cancerous and noncancerous tumors displayed remarkable haptically distinguishable differences in their material toughness.

Conclusion

The qualitative method described here, though subject to some operator bias, identifies a previously unreported in vivo approach to classify fracture toughness of a solid tumor that can be correlated with malignancy, and paves the way for the development of a mechanical device that can accurately quantify the tissue toughness of a human tumor.     

Static versus dynamic gerbil tympanic membrane elasticity: derivation of the complex modulus

An accurate estimation of tympanic membrane stiffness is important for realistic modelling of middle ear mechanics. Tympanic membrane stiffness has been investigated extensively under either quasi-static or dynamic loading conditions. It is known that biological tissues are sensitive to strain rate. Therefore, in this work, the mechanical behaviour of the tympanic membrane was studied under both quasi-static and dynamic loading conditions. Experiments were performed on the pars tensa of four gerbil tympanic membranes. A custom-built indentation apparatus was used to perform in situ tissue indentations and testing was done applying both quasi-static and dynamic sinusoidal indentations up to 8.2?Hz. The unloaded shape of the tympanic membrane was measured and used to create specimen-specific finite element models to simulate the experiments. The frequency dependent Young's modulus of each specimen was then estimated by an inverse analysis in which the error between experimental and simulated indentation data was optimised for each indentation frequency separately. Using an 8?μm central region thickness, we found Young's moduli between 71 and 106?MPa (n = 4) at 0.2?Hz indentation frequency. A standard linear viscoelastic model and a viscoelastic model with a continuous relaxation spectrum were used to derive a complex modulus in the frequency domain. Due to experimental limitations, the indentation frequency upper limit was 8.2?Hz. The average relative modulus increase in this domain was 14% and the increase was the strongest below 6?Hz.     

Derivation of the Stress-Strain Behavior of the constituents of Bio-Inspired Layered TiO₂/PE-Nanocomposites by Inverse Modeling Based on FE-Simulations of Nanoindentation Test

Owing to the apparent simple morphology and peculiar properties, nacre, an iridescent layer, coating of the inner part of mollusk shells, has attracted considerable attention of biologists, material scientists and engineers. The basic structural motif in nacre is the assembly of oriented plate-like aragonite crystals with a ’brick’ (CaCO₃ crystals) and ’mortar’ (macromolecular components like proteins) organization. Many scientific researchers recognize that such structures are associated with the excellent mechanical properties of nacre and biomimetic strategies have been proposed to produce new layered nanocomposites. During the past years, increasing efforts have been devoted towards exploiting nacre’s structural design principle in the synthesis of novel nanocomposites. However, the direct transfer of nacre’s architecture to an artificial inorganic material has not been achieved yet. In the present contribution we report on laminated architecture, composed of the inorganic oxide (TiO₂) and organic polyelectrolyte (PE) layers which fulfill this task.
To get a better insight and understanding concerning the mechanical behaviour of bio-inspired layered materials consisting of oxide ceramics and organic layers, the elastic-plastic properties of titanium dioxide and organic polyelectrolyte phase are determined via FE-modelling of the nanoindentation process. With the use of inverse modeling and based on numerical models which are applied on the microscopic scale, the material properties of the constituents are derived.     

Some mechanical properties of crossed fibrillar chitin

The sclerites of P. sinuata consist of crossed reticulate layers of chitin fibrils arranged in the preferred orientation together with protein glues. Stretched beetle whole cuticle and chitin obey Hooke's law in the elastic region. Anisotropic swelling in a sclerite ensures flexibility and prevents sliding in the plane surface. Chitin micelle orientation can be strain-induced in vitro. Although two-phase materials, neither beetle nor locust cuticle meet the requirements of plywood mechanics.     

Nanomechanical Behaviours of Cuticle of Three Kinds of Beetle

The surface materials and structures of insect cuticle can provide useful information for designing anti-adhesion components material. Quantitative measurement of mechanical properties of insect cuticle will help to develop biomimetic materials suitable for industrial products. In this work, the mechanical properties, such as the reduced modulus and hardness in nano-scale, of the cuticle of beetle Geotrupes stercorarius Linnaeus, Copris ochus Motschulsky and Holotrichia sichotana Brenske, were investigated by using a nanoindenter. It was found that the reduce modulus and hardness of these three beetles are different. The main cause of the difference of the mechanical properties is probably due to their different living circumstance, lifestyle and different functions of segments.     

The toughness of secondary cell wall and woody tissue

The ''across grain'' toughness of 51 woods has been determined on thin wet sections using scissors. The moisture content of sections and the varying sharpness of the scissor blades had little effect on the results. In thin sections (less than 0.6mm), toughness rose linearly with section thickness. The intercept toughness at zero thickness, estimated from regression analysis, was proportional to relative density, consistent with values reported for non-woody plant tissues. Extrapolation of the intercept toughness of these woods and other plant tissues/materials to a relative density of 1.0 predicted a toughness of 3.45kJ m^-2 , which we identify with the intrinsic toughness of the cell wall. This quantity appears to predict published results from K_IC tests on woods and is related to the propensity for crack deflection. The slope of the relationship between section thickness and toughness, describing the work of plastic buckling of cells, was not proportional to relative density, the lightest (balsa) and heaviest (lignum vitae) woods fracturing with less plastic work than predicted. The size of the plastic zone around the crack tip was estimated to be 0.5mm in size. From this, the hypothetical overall toughness of a thick (greater than 1 mm) block of solid cell wall material was calculated as 39.35 kJ m^-2, due to both cell wall resistance (10 per cent) and the plastic buckling of cells (90 per cent). This value successfully predicts the toughness of most commercial woods (of relative densities between 0.2 and 0.8) from ''work area'' tests in tension and bending. Though density was the most important factor, both fibre width/fibre length (in hardwoods) and lignin/cellulose ratios were negatively correlated with the work of plastic buckling, after correcting for density. At low densities the work of plastic buckling in the longitudinal radial (LR) direction exceeded that in longitudinal tangential (LT), but the reverse was true for relative densities above 0.25. This could be attributed to the direction of rays. Density for density, the toughness of temperate hardwoods tested was about 20 per cent lower than that of tropical hardwoods. This is probably due to the much greater number of vessels in temperate hardwoods. Vessels appear either not to display buckling behaviour during fracture at all or to collapse cheaply. These general results have applications to other plant tissues.     

Comparison of elastic,viscoelastic and failure tensile material properties of knee ligaments and patellar tendon

The knee ligaments and patellar tendon function in concert with each other and other joint tissues, and are adapted to their specific physiological function via geometry and material properties. However, it is not well known how the viscoelastic and quasi-static material properties compare between the ligaments. The purpose of this study was to characterize and compare these material properties between the knee ligaments and patellar tendon.Dumbbell-shaped tensile test samples were cut from bovine knee ligaments (ACL, LCL, MCL, PCL) and patellar tendon (PT) and subjected to tensile testing (n = 10 per ligament type). A sinusoidal loading test was performed at 8% strain with 0.5% strain amplitude using 0.1, 0.5 and 1 Hz frequencies. Subsequently, an ultimate tensile test was performed to investigate the stress-strain characteristics.At 0.1 Hz, the phase difference between stress and strain was higher in LCL compared with ACL, PCL and PT (p < 0.05), and at 0.5 Hz that was higher in LCL compared with all other ligaments and PT (p < 0.05). PT had the longest toe-region strain (p < 0.05 compared with PCL and MCL) and MCL had the highest linear and strain-dependent modulus, and toughness (p < 0.05 compared with ACL, LCL and PT).The results indicate that LCL is more viscous than other ligaments at low-frequency loads. MCL was the stiffest and toughest, and its modulus increased most steeply at the toe-region, possibly implying a greater amount of collagen. This study improves the knowledge about elastic, viscoelastic and failure properties of the knee ligaments and PT.     

Foliar secretory trichomes of Ocimum obovatum (Lamiaceae): micromorphological structure and histochemistry

This study characterises the micromorphology, ultrastructure and main chemical constituents of the foliar glandular trichomes of Ocimum obovatum using light and electron microscopy and a variety of histochemical tests. Two types of glandular trichomes occur on the leaves: large peltate and small capitate. The head of each peltate trichome is made up of four broad head cells in one layer. The head of each capitate trichome is composed of two broad head cells in one layer (type I) or a single oval head cell (type II, rare). In peltate heads, secretory materials are gradually transported to the subcuticular space via fracture in the four sutures at the connecting walls of the head cells. Release to the head periphery occurs through opposite fracture in the four sutures in the head cuticle. In type I capitate trichomes, release of the secretions to the subcuticular space occurs via a pore between the two head cells, and release to the head periphery occurs through the opposite pore in the head cuticle. In type II capitate trichomes, the secreted material is released from the head cell through a ruptured particular squared area at the central part of the head cuticle. These secretion modes are reported for the first time in the family Lamiaceae. Histochemical tests showed that the secretory materials in the glandular trichomes are mainly essential oils, lipophilic substances and polysaccharides. Large peltate trichomes contain a large quantity of these substances than the small capitate trichomes. Ultrastructural evidence suggests that the plastids produce numerous lipid droplets, and the numerous polysaccharide small vesicles are derived from Golgi bodies.     

Factors impacting nanoindentation testing results of the cuticle of dung beetle Copris ochus Motschulsky

1 Introduction Insects have been adapted to their living surround-ings. Two different adaptations they have were the pas-sive adaptation and the active adaptation. For examples,the passive adaptation of soil insects to the soil habitatresulted in shorter or vestigial additional legs, the bodybecoming smaller, thinner or flatter, and wings and eyesdiminishing; the stronger digging legs of some soil in-sects were a result of active adaptation for burrowing [1]. The biological character…     

Application of fracture mechanics to failure in manatee rib bone

BACKGROUND: The Florida manatee (Trichechus manatus latirostris) is listed as endangered by the U.S. Department of the Interior. Manatee ribs have different microstructure from the compact bone of other mammals. Biomechanical properties of the manatee ribs need to be better understood. Fracture toughness (K(C)) has been shown to be a good index to assess the mechanical performance of bone. Quantitative fractography can be used in concert with fracture mechanics equations to identify fracture initiating defects/cracks and to calculate the fracture toughness of bone materials. METHOD OF APPROACH: Fractography is a standard technique for analyzing fracture behavior of brittle and quasi-brittle materials. Manatee ribs are highly mineralized and fracture in a manner similar to quasi-brittle materials. Therefore, quantitative fractography was applied to determine the fracture toughness of manatee ribs. RESULTS: Average fracture toughness values of small flexure specimens from six different sizes of manatees ranged from 1.3 to 2.6 MPa(m)(12). Scanning electron microscope (SEM) images show most of the fracture origins were at openings for blood vessels and interlayer spaces. CONCLUSIONS: Quantitative fractography and fracture mechanics can be combined to estimate the fracture toughness of the material in manatee rib bone. Fracture toughness of subadult and calf manatees appears to increase as the size of the manatee increases. Average fracture toughness of the manatee rib bone materials is less than the transverse fracture toughness of human and bovine tibia and femur.     

Evaluation of fracture toughness of human dentin using elastic-plastic fracture mechanics

Dentin, the mineralized tissue forming the bulk of the tooth, lies between the enamel and the pulp chamber. It is a rich source of inspiration for designing novel synthetic materials due to its unique microstructure. Most of the previous studies investigating the fracture toughness of dentin have used linear-elastic fracture mechanics (LEFM) that ignores plastic deformation and could underestimate the toughness of dentin. With the presence of collagen (approximately 30% by volume) aiding the toughening mechanisms in dentin, we hypothesize that there is a significant difference between the fracture toughness estimated using LEFM (Kc) and elastic-plastic fracture mechanics (EPFM) (KJc). Single-edge notched beam specimens with in-plane (n=10) and anti-plane (n=10) parallel fractures were prepared following ASTM standard E1820 and tested in three-point flexure. KJc of the in-plane parallel and anti-plane parallel specimens were found to be 3.1 and 3.4 MPa m 1/2 and Kc were 2.4 and 2.5 MPa m 1/2, respectively. The fracture toughness estimated based on KJc is significantly greater than that estimated based on Kc (32.5% on average; p<0.001). In addition, KJc of anti-plane parallel specimens is significantly greater than that of in-plane parallel specimens. We suggest that, in order to critically evaluate the fracture toughness of human dentin, EPFM should be employed.