Multiscale structure and damage tolerance of coconut shells.

We investigated the endocarp of the fruit of Cocos nucifera (i.e., the inner coconut shell), examining the structure across multiple length scales through advanced characterization techniques and in situ testing of mechanical properties. Like many biological materials, the coconut shell possesses a hierarchical structure with distinct features at different length scales that depend on orientation and age. Aged coconut was found to have a significantly stronger (ultimate tensile strength, UTS = 48.5MPa), stiffer (Young's modulus, E = 1.92GPa), and tougher (fracture resistance (R-curve) peak of KJ = 3.2MPa m1/2) endocarp than the younger fruit for loading in the latitudinal orientation. While the mechanical properties of coconut shell were observed to improve with age, they also become more anisotropic: the young coconut shell had the same strength (17MPa) and modulus (0.64GPa) values and similar R-curves for both longitudinal and latitudinal loading configurations, whereas the old coconut had 82% higher strength for loading in the latitudinal orientation, and >50% higher crack growth toughness for cracking on the latitudinal plane. Structural aspects affecting the mechanical properties across multiple length scales with aging were identified as improved load transfer to the cellulose crystalline nanostructure (identified by synchrotron x-ray diffraction) and sclerification of the endocarp, the latter of which included closing of the cell lumens and lignification of the cell walls. The structural changes gave a denser and mechanically superior micro and nanostructure to the old coconut shell. Additionally, the development of anisotropy was attributed to the formation of an anisotropic open channel structure throughout the shell of the old coconut that affected both crack initiation during uniaxial tensile tests and the toughening mechanisms of crack trapping and deflection during crack propagation.

Kitagawa-Takahashi diagrams define the limiting conditions for cyclic fatigue failure in human dentin.

As cyclic fatigue is considered to be a major cause of clinical tooth fractures, achieving a comprehensive understanding of the fatigue behavior of dentin is of importance. In this note, the fatigue behavior of human dentin is examined in the context of the Kitagawa-Takahashi diagram to define the limiting conditions for fatigue failure. Specifically, this approach incorporates two limiting threshold criteria for fatigue: (i) a threshold stress for fatigue failure, specifically the smooth-bar (unnotched) fatigue endurance strength, at small crack sizes and (ii) a threshold stress-intensity range for fatigue-crack growth at larger crack sizes. The approach provides a "bridge" between the traditional fatigue life and fracture mechanics based damage-tolerant approaches to fatigue-life estimation, and as such defines a "failure envelope" of applied stresses and flaw sizes where fatigue failure is likely in dentin This approach may also be applied to fatigue failure in human cortical bone (i.e. clinical "stress fractures"), which exhibits similar fatigue behavior characteristics, and in principle may aid clinicians in making quantitative evaluations of the risk of fractures in mineralized tissues.

Propagation of surface fatigue cracks in human cortical bone.

An understanding of how fatigue cracks grow in bone is of importance as fatigue is thought to be the main cause of clinical stress fractures. This study presents new results on the fatigue-crack growth behavior of small surface cracks (approximately 75-1000 microm in size) in human cortical bone, and compares their growth rates with data from other published studies on the behavior of both surface cracks and many millimeter, through-thickness large cracks. Results are obtained with a cyclically loaded cantilever-beam geometry using optical microscopy to examine for crack growth after every 100-500 cycles. Based on the current and previous results, small fatigue cracks appear to become more resistant to fatigue-crack growth with crack extension, analogous to the way the fracture resistance of cortical bone increases with crack growth. Mechanistically, a theory attributing such behavior to the development of bridges in the wake of the crack with crack growth is presented. The existence of such bridges is directly confirmed using optical microscopy.

Bioactive glass fillers reduce bacterial penetration into marginal gaps for composite restorations.

OBJECTIVE: Bioactive glass (BAG) is known to possess antimicrobial and remineralizing properties; however, the use of BAG as a filler for resin based composite restorations to slow recurrent caries has not been studied. Accordingly, the objective of this study was to investigate the effect of adding 15wt% BAG to a resin composite on bacterial biofilms penetrating into marginal gaps of simulated tooth fillings in vitro during cyclic mechanical loading. METHODS: Human molars were machined into approximately 3mm thick disks of dentin and 1.5-2mm deep composite restorations were placed. A narrow 15-20 micrometer wide dentin-composite gap was allowed to form along half of the margin by not applying dental adhesive to that region. Two different 72wt% filled composites were used, one with 15wt% BAG filler (15BAG) and the balance silanated strontium glass and one filled with aerosol silica and silanated strontium glass without BAG (0BAG-control). Samples of both groups had Streptococcus mutans biofilms grown on the surface and were tested inside a bioreactor for two weeks while subjected to periods of cyclic mechanical loading. After post-test biofilm viability was confirmed, each specimen was fixed in glutaraldehyde, gram positive stained, mounted in resin and cross-sectioned to reveal the gap profile. Depth of biofilm penetration for 0BAG and 15BAG was quantified as the fraction of gap depth. The data were compared using a Student's t-test. RESULTS: The average depth of bacterial penetration into the marginal gap for the 15BAG samples was significantly smaller (∼61%) in comparison to 0BAG, where 100% penetration was observed for all samples with the biofilm penetrating underneath of the restoration in some cases. SIGNIFICANCE: BAG containing resin dental composites reduce biofilm penetration into marginal gaps of simulated tooth restorations. This suggests BAG containing composites may have the potential to slow the development and propagation of secondary tooth decay at restoration margins.

Mechanistic aspects of in vitro fatigue-crack growth in dentin.

Although the propagation of fatigue cracks has been recognized as a problem of clinical significance in dentin, there have been few fracture mechanics-based studies that have investigated this issue. In the present study, in vitro cyclic fatigue experiments were conducted over a range of cyclic frequencies (1-50 Hz) on elephant dentin in order to quantify fatigue-crack growth behavior from the perspective of understanding the mechanism of fatigue in dentin. Specifically, results obtained for crack extension rates along a direction parallel to the dentinal tubules were found to be well described by the stress-intensity range, DeltaK, using a simple Paris power-law approach with exponents ranging from 12 to 32. Furthermore, a frequency dependence was observed for the crack-growth rates, with higher growth rates associated with lower frequencies. By using crack-growth experiments involving alternate cyclic and static loading, such fatigue-crack propagation was mechanistically determined to be the result of a "true" cyclic fatigue mechanism, and not simply a succession of static fracture events. Furthermore, based on the observed frequency dependence of fatigue-crack growth in dentin and observations of time-dependent crack blunting, a cyclic fatigue mechanism involving crack-tip blunting and re-sharpening is proposed. These results are deemed to be of importance for an improved understanding of fatigue-related failures in teeth.

Mechanistic aspects of fracture and R-curve behavior in human cortical bone.

An understanding of the evolution of toughness is essential for the mechanistic interpretation of the fracture of cortical bone. In the present study, in vitro fracture experiments were conducted on human cortical bone in order to identify and quantitatively assess the salient toughening mechanisms. The fracture toughness was found to rise linearly with crack extension (i.e., rising resistance- or R-curve behavior) with a mean crack-initiation toughness, K0 of approximately 2 MPa square root m for crack growth in the proximal-distal direction. Uncracked ligament bridging, which was observed in the wake of the crack, was identified as the dominant toughening mechanism responsible for the observed R-curve behavior. The extent and nature of the bridging zone was examined quantitatively using multi-cutting compliance experiments in order to assess the bridging zone length and estimate the bridging stress distribution. Additionally, time-dependent cracking behavior was observed at stress intensities well below those required for overload fracture; specifically, slow crack growth occurred at growth rates of approximately 2 x 10(-9) m/s at stress intensities approximately 35% below the crack-initiation toughness. In an attempt to measure slower growth rates, it was found that the behavior switched to a regime dominated by time-dependent crack blunting, similar to that reported for dentin; however, such blunting was apparent over much slower time scales in bone, which permitted subcritical crack growth to readily take place at higher stress intensities.

Aspects of in vitro fatigue in human cortical bone: time and cycle dependent crack growth.

Although fatigue damage in bone induced by cyclic loading has been recognized as a problem of clinical significance, few fracture mechanics based studies have investigated how incipient cracks grow by fatigue in this material. In the present study, in vitro cyclic fatigue experiments were performed in order to quantify fatigue-crack growth behavior in human cortical bone. Crack-growth rates spanning five orders of magnitude were obtained for the extension of macroscopic cracks in the proximal-distal direction; growth-rate data could be well characterized by the linear-elastic stress-intensity range, using a simple (Paris) power law with exponents ranging from 4.4 to 9.5. Mechanistically, to discern whether such behavior results from "true" cyclic fatigue damage or is simply associated with a succession of quasi-static fracture events, cyclic crack-growth rates were compared to those measured under sustained (non-cyclic) loading. Measured fatigue-crack growth rates were found to exceed those "predicted" from the sustained load data at low growth rates ( approximately 3 x 10(-10) to 5 x 10(-7) m/cycle), suggesting that a "true" cyclic fatigue mechanism, such as alternating blunting and re-sharpening of the crack tip, is active in bone. Conversely, at higher growth rates ( approximately 5 x 10(-7) to 3 x 10(-5) m/cycle), the crack-growth data under sustained loads integrated over the loading cycle reasonably predicts the cyclic fatigue data, indicating that quasi-static fracture mechanisms predominate. The results are discussed in light of the occurrence of fatigue-related stress fractures in cortical bone.

Simple and accurate fracture toughness testing methods for pyrolytic carbon/graphite composites used in heart-valve prostheses.

The fracture toughness is a critical material property for the pyrolytic carbon materials used in mechanical heart-valve prostheses; however, making accurate toughness measurements has traditionally been problematic due to difficulties in fatigue precracking specimens. In this work, a simple, effective, and reliable precracking method is presented where a sharp precrack is "popped in" from a razor micronotch, which allows significant savings of time and materials relative to fatigue precracking methods. It is further shown that equivalent results may be obtained using razor micronotched specimens directly without precracking, provided the notch is sufficiently sharp. Indeed, mean toughness values of 1.46+/-0.13 and 1.35+/-0.09 MPa radicalm were obtained for the pyrolytic carbon-coated graphite materials, using precracked and razor micronotched specimens, respectively. The difference between these mean values proved to be statistically insignificant, and these values are in general agreement with published fracture toughness results obtained using fatigue precracked specimens.

Effects of polar solvents on the fracture resistance of dentin: role of water hydration.

Although healthy dentin is invariably hydrated in vivo, from a perspective of examining the mechanisms of fracture in dentin, it is interesting to consider the role of water hydration. Furthermore, it is feasible that exposure to certain polar solvents, e.g., those found in clinical adhesives, can induce dehydration. In the present study, in vitro deformation and fracture experiments, the latter involving a resistance-curve (R-curve) approach (i.e., toughness evolution with crack extension), were conducted in order to assess changes in the constitutive and fracture behavior induced by three common solvents-acetone, ethanol and methanol. In addition, nanoindentation-based experiments were performed to evaluate the deformation behavior at the level of individual collagen fibers and ultraviolet Raman spectroscopy to evaluate changes in bonding. The results indicate a reversible effect of chemical dehydration, with increased fracture resistance, strength, and stiffness associated with lower hydrogen bonding ability of the solvent. These results are analyzed both in terms of intrinsic and extrinsic toughening phenomena to further understand the micromechanisms of fracture in dentin and the specific role of water hydration.

Cyclic mechanical loading promotes bacterial penetration along composite restoration marginal gaps.

OBJECTIVES: Secondary caries is the most common reason for composite restoration replacement and usually forms between dentin and the filling. The objective of this study was to investigate the combined effect of cyclic loading and bacterial exposure on bacterial penetration into gaps at the interface between dentin and resin composite restorative material using a novel bioreactor system and test specimen design. METHODS: Human molars were machined into 3mm thick disks with 2mm deep × 5 mm diameter cavity preparations into which composite restorations were placed. A ∼ 15-30 µm (small) or ∼ 300 µm wide (large) marginal gap was introduced along half of the interface between the dentin and restoration. Streptococcus mutans UA 159 biofilms were grown on each sample prior to testing each in a bioreactor both with and without cyclic loading. Both groups of samples were tested for 2 weeks and post-test biofilm viability was confirmed with a live-dead assay. Samples were fixed, mounted and cross-sectioned to reveal the gaps and observe the depth of bacterial penetration. RESULTS: It was shown that for large gap samples the bacteria easily penetrated to the full depth of the gap independent of loading or non-loading conditions. The results for all cyclically loaded small gap samples show a consistently deep bacterial penetration down 100% of the gap while the average penetration depth was only 67% for the non-loaded samples with only two of six samples reaching 100%. SIGNIFICANCE: A new bioreactor was developed that allows combining cyclic mechanical loading and bacterial exposure of restored teeth for bacterial biofilm and demineralization studies. Cyclic loading was shown to aid bacterial penetration into narrow marginal gaps, which could ultimately promote secondary caries formation.

On the origin of the toughness of mineralized tissue: microcracking or crack bridging?

Two major mechanisms that could potentially be responsible for toughening in mineralized tissues, such as bone and dentin, have been identified-microcracking and crack bridging. While evidence has been reported for both mechanisms, there has been no consensus thus far on which mechanism plays the dominant role in toughening these materials. In the present study, we seek to present definitive experimental evidence supporting crack bridging, rather than microcracking, as the most significant mechanism of toughening in cortical bone and dentin. In vitro fracture toughness experiments were conducted to measure the variation of the fracture resistance with crack extension [resistance-curve (R-curve) behavior] for both materials with special attention paid to changes in the sample compliance. Because these two toughening mechanisms induce opposite effects on the sample compliance, such experiments allow for the definitive determination of the dominant toughening mechanism, which in the present study was found to be crack bridging for microstructurally large crack sizes. The results of this work are of relevance from the perspective of developing a micromechanistic framework for understanding fracture behavior of mineralized tissue and in predicting failure in vivo.

Effect of aging on the toughness of human cortical bone: evaluation by R-curves.

Age-related deterioration of the fracture properties of bone, coupled with increased life expectancy, is responsible for increasing incidence of bone fracture in the elderly, and hence, an understanding of how its fracture properties degrade with age is essential. The present study describes ex vivo fracture experiments to quantitatively assess the effect of aging on the fracture toughness properties of human cortical bone in the longitudinal direction. Because cortical bone exhibits rising crack-growth resistance with crack extension, unlike most previous studies, the toughness is evaluated in terms of resistance-curve (R-curve) behavior, measured for bone taken from wide range of age groups (34-99 years). Using this approach, both the ex vivo crack-initiation and crack-growth toughness are determined and are found to deteriorate with age; the initiation toughness decreases some 40% over 6 decades from 40 to 100 years, while the growth toughness is effectively eliminated over the same age range. The reduction in crack-growth toughness is considered to be associated primarily with a degradation in the degree of extrinsic toughening, in particular, involving crack bridging in the wake of the crack.

Crack blunting, crack bridging and resistance-curve fracture mechanics in dentin: effect of hydration.

Few studies have focused on a description of the fracture toughness properties of dentin in terms of resistance-curve (R-curve) behavior, i.e., fracture resistance increasing with crack extension, particularly in light of the relevant toughening mechanisms involved. Accordingly, in the present study, fracture mechanics based experiments were conducted on elephant dentin in order to determine such R-curves, to identify the salient toughening mechanisms and to discern how hydration may affect their potency. Crack bridging by uncracked ligaments, observed directly by microscopy and X-ray tomography, was identified as a major toughening mechanism, with further experimental evidence provided by compliance-based experiments. In addition, with hydration, dentin was observed to display significant crack blunting leading to a higher overall fracture resistance than in the dehydrated material. The results of this work are deemed to be of importance from the perspective of modeling the fracture behavior of dentin and in predicting its failure in vivo.

An inset CT specimen for evaluating fracture in small samples of material.

In evaluations on the fracture behavior of hard tissues and many biomaterials, the volume of material available to study is not always sufficient to apply a standard method of practice. In the present study an inset Compact Tension (inset CT) specimen is described, which uses a small cube of material (approximately 2×2×2mm(3)) that is molded within a secondary material to form the compact tension geometry. A generalized equation describing the Mode I stress intensity was developed for the specimen using the solutions from a finite element model that was defined over permissible crack lengths, variations in specimen geometry, and a range in elastic properties of the inset and mold materials. A validation of the generalized equation was performed using estimates for the fracture toughness of a commercial dental composite via the "inset CT" specimen and the standard geometry defined by ASTM E399 (2006). Results showed that the average fracture toughness obtained from the new specimen (1.23±0.02MPam(0.5)) was within 2% of that from the standard. Applications of the inset CT specimen are presented for experimental evaluations on the crack growth resistance of dental enamel and root dentin, including their fracture resistance curves. Potential errors in adopting this specimen are then discussed, including the effects of debonding between the inset and molding material on the estimated stress intensity distribution. Results of the investigation show that the inset CT specimen offers a viable approach for studying the fracture behavior of small volumes of structural materials.

Mechanical performance of novel bioactive glass containing dental restorative composites.

OBJECTIVES: Bioactive glass (BAG) is known to possess antimicrobial properties and release ions needed for remineralization of tooth tissue, and therefore may be a strategic additive for dental restorative materials. The objective of this study was to develop BAG containing dental restorative composites with adequate mechanical properties comparable to successful commercially available composites, and to confirm the stability of these materials when exposed to a biologically challenging environment. METHODS: Composites with 72 wt% total filler content were prepared while substituting 0-15% of the filler with ground BAG. Flexural strength, fracture toughness, and fatigue crack growth tests were performed after several different soaking treatments: 24h in DI water (all experiments), two months in brain-heart infusion (BHI) media+Streptococcus mutans bacteria (all experiments) and two months in BHI media (only for flexural strength). Mechanical properties of new BAG composites were compared along with the commercial composite Heliomolar by two-way ANOVA and Tukey's multiple comparison test (p≤0.05). RESULTS: Flexural strength, fracture toughness, and fatigue crack growth resistance for the BAG containing composites were unaffected by increasing BAG content up to 15% and were superior to Heliomolar after all post cure treatments. The flexural strength of the BAG composites was unaffected by two months exposure to aqueous media and a bacterial challenge, while some decreases in fracture toughness and fatigue resistance were observed. The favorable mechanical properties compared to Heliomolar were attributed to higher filler content and a microstructure morphology that better promoted the toughening mechanisms of crack deflection and bridging. SIGNIFICANCE: Overall, the BAG containing composites developed in this study demonstrated adequate and stable mechanical properties relative to three successful commercial composites.

Mechanistic aspects of fatigue crack growth behavior in resin based dental restorative composites.

OBJECTIVE: To test the hypothesis that a commercial microhybrid resin based composite (Filtek Z250) has superior fatigue resistance to a nanofill composite (Filtek Supreme Plus) and to determine the related micromechanisms involved in the fatigue process. METHODS: After 60 days of water hydration, the fatigue crack growth resistance of two different resin composites, one microhybrid (Filtek Z250) and one nanofill (Filtek Supreme Plus), was measured in wet conditions using compact-tension, C(T), specimens at a load ratio of 0.1 and frequency of 2Hz. Cyclic fatigue behavior was quantified in terms of the fatigue crack growth rate, da/dN, as a function of the stress intensity range, DeltaK. RESULTS: A sigmoidal da/dN-DeltaK curve with three different fatigue crack growth regimes was identified for both composites. In general, fatigue crack growth ranged from approximately 10(-9) to 10(-5)m/cycle over DeltaK of 0.54-0.63MPa radicalm for the Z250 composite and DeltaK of 0.41-0.67MPa radicalm for the Supreme Plus composite. The Supreme Plus composite showed a lower fatigue threshold, DeltaK(th), by approximately 0.13MPa radicalm compared to the Z250 composite, while also showing a plateau in the fatigue crack growth curve that is likely related to environmental attack. SEM observations of the fatigue crack paths and fracture surfaces revealed an interparticle crack path and extrinsic toughening mechanisms of crack deflection and crack bridging. No fatigue degradation of reinforcing particles or clusters was found, but cluster-matrix debonding was evident in the Supreme Plus composite, also indicative of environmental attack due to water. SIGNIFICANCE: This study increases the understanding of both the fatigue behavior and the micromechanisms of fatigue in resin based dental composites.

R-curve behavior and toughening mechanisms of resin-based dental composites: effects of hydration and post-cure heat treatment.

OBJECTIVES: To test the hypothesis that the fracture resistance of two different particulate resin composites degrade after water hydration and improve after post-cure heat treatment, and to correlate those changes with salient failure micromechanisms. METHODS: Two composites with different filler morphology were selected, denoted microhybrid (Filtek Z250) and nanofill (Filtek Supreme plus). Following initial light curing, hydrated samples were aged in water for 60 days at room temperature while post-cured samples were heat treated at 120 degrees C for 90 min. Fracture resistance was assessed using fracture resistance curves (R-curves) utilizing pre-cracked compact tension, C(T), specimens. The flexural strength of the hydrated composites also was evaluated in four-point bending using unnotched beams. Scanning electron microscopy (SEM) of crack paths and fracture surfaces was performed to determine the micromechanisms of fracture and toughening. The results were compared by two-way ANOVA and Tukey's multiple comparison test (p< or =0.05). RESULTS: SEM observations revealed a predominantly interparticle matrix crack path for all cases except the hydrated nanofill composite, which showed evidence of particle matrix debonding. Hydration lowered the strength for both composites and the peak toughness for the nanofill composite. The strength decrease was attributed to resin matrix plasticization and hydrolytic degradation in both cases, with additional interfacial degradation causing a larger strength decline and concomitant peak toughness decrease in the nanofill composite. The post-cure heat treatment noticeably changed the R-curve shape causing the peak toughness to be reached after shorter amounts of crack extension. Such changes help explain the increases in strength reported in other studies and is attributed to improved resin matrix properties. SIGNIFICANCE: Results from this study provide new insight into the micromechanisms of fracture in resin-based dental composites which should aid the future development and improvement of these materials.

Indentation techniques for evaluating the fracture toughness of biomaterials and hard tissues.

Indentation techniques for assessing fracture toughness are attractive due to the simplicity and expediency of experiments, and because they potentially allow the characterization of both local and bulk fracture properties. Unfortunately, rarely have such techniques been proven to give accurate fracture toughness values. This is a concern, as such techniques are seeing increasing usage in the study of biomaterials and biological hard tissues. Four available indentation techniques are considered in the present article: the Vickers indentation fracture (VIF) test, the cube corner indentation fracture (CCIF) test, the Vickers crack opening displacement (VCOD) test and the interface indentation fracture (IIF) test. Each technique is discussed in terms of its suitability for assessing the absolute and relative toughness of materials or material interfaces based on the published literature on the topic. In general, the VIF and CCIF techniques are found to be poor for quantitatively evaluating toughness of any brittle material, and the large errors involved (approximately +/-50%) make their applicability as comparative techniques limited. Indeed, indentation toughness values must differ by at least by a factor of three to conclude a significant difference in actual toughness. Additionally, new experimental results are presented on using the CCIF test to evaluate the fracture resistance of human cortical bone. Those new results indicate that inducing cracking is difficult, and that the cracks that do form are embedded in the plastic zone of the indent, invalidating the use of linear elastic fracture mechanics based techniques for evaluating the toughness associated with those cracks. The VCOD test appears to be a good quantitative method for some glasses, but initial results suggest there may be problems associated with applying this technique to other brittle materials. Finally, the IIF technique should only be considered a comparative or semi-quantitative technique for comparing material interfaces and/or the neighboring materials.

R-curve behavior and micromechanisms of fracture in resin based dental restorative composites.

The fracture properties and micromechanisms of fracture for two commercial dental composites, one microhybrid (FiltekZ250) and one nanofill (FiltekSupreme Plus), were studied by measuring fracture resistance curves (R-curves) using pre-cracked compact-tension specimens and by conducting both unnotched and double notched four point beam bending experiments. Four point bending experiments showed about 20% higher mean flexural strength of the microhybrid composite compared to the nanofill. Rising fracture resistance was observed over approximately 1 mm of crack extension for both composites, and higher overall fracture resistance was observed for the microhybrid composite. Such fracture behavior was attributed to crack deflection and crack bridging toughening mechanisms that developed with crack extension, causing the toughness to increase. Despite the lower strength and toughness of the present nanofill composite, based on micromechanics observations, large nanoparticle clusters appear to be as effective at deflecting cracks and imparting toughening as solid particles. Thus, with further microstructural refinement, it should be possible to achieve a superior combination of aesthetic and mechanical performance using the nanocluster approach for dental composites.