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.     

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.     

Fracture toughness of human dentin

The purpose of this study was to determine the fracture toughness (K(IC)) of human dentin and to test the null hypothesis that K(IC) is not affected by the orientation of dentinal tubules relative to the plane of crack propagation. Triangular prisms (4 x 4 x 4 x 8 mm) were obtained from human molars and tested using the notchless triangular prism (NTP) specimen K(IC) test. Dentin prisms were prepared so that the plane of crack propagation would have three different orientations relative to the orientation of dentinal tubules: perpendicular (PE), parallel aligned (PAA), and parallel transverse (PAT). The prepared specimens were secured in the specimen holder and loaded in tension until fracture or crack arrest. The maximum load recorded was used to calculate K(IC). There was no significant difference between the K(IC) of PAA specimens (1.97 +/- 0.17 MPa/m(1/2)) and PAT (2.02 +/- 0.18 MPa/m(1/2)). The K(IC) for the PE specimens (1.13 +/- 0.36 MPa/m(1/2)) was significantly lower. The SEM images of the fractured surfaces showed distinct differences that were correlated with the determined K(IC) values. The fractured surfaces of PAA and PAT specimens were rougher compared to PE specimens. Both the hyper mineralized peritubular dentin and the orientation of collagen fibrils surrounding the tubules could be responsible for the significant differences in K(IC). The results of this study identified a significant anisotropy of dentin with respect to its K(IC).     

年龄变化对人牙本质裂纹扩展升阻能力的影响

目的通过有限元数值计算的方法研究年龄变化对牙本质断裂力学行为的影响。方法根据典型的紧凑拉伸试件形式建立有限元模型,采用内聚力模型分别模拟裂纹在年轻和老龄牙本质中稳态扩展的过程,并进行比较。结果老龄牙本质的扩展断裂韧度和断裂韧度趋于恒定时的值分别为0.51、1.19 MPa.m1/2,显著小于年轻牙本质的相应值(7.48、1.71 MPa.m1/2);然而,这两者之间的初始断裂韧度相差比较微小,年轻和老龄牙本质的初始断裂韧度分别为0.51和0.38 MPa.m1/2。结论随着年龄的增长,牙本质抵抗裂纹扩展的能力发生了明显的减弱。基于内聚力模型的数值方法能够很好地预测牙本质等力学性能与年龄相关的生物硬组织材料的裂纹扩展行为。     

Tubule orientation and the fatigue strength of human dentin

In this study the influence of tubule orientation on the strength of human dentin under static and cyclic loads was examined. Rectangular beams were sectioned from the coronal dentin of virgin extracted molars (N=83) and then loaded in quasi-static 4-point flexure or 4-point flexural fatigue to failure. The flexure strength, energy to fracture and fatigue strength were evaluated for specimens with the dentin tubules aligned parallel (theta=0 degrees ) and perpendicular (theta=90 degrees ) to the plane of maximum normal stress. Results from monotonic loading showed that both the flexural strength and energy to fracture of dentin specimens with theta=0 degrees were significantly greater than those with theta=90 degrees . Furthermore, the apparent endurance strength of dentin with theta=0 degrees (44MPa) was significantly greater than that of the dentin with theta=90 degrees (24MPa). The ratio of apparent endurance strength (for fully reversed loading) to the flexure strength for theta=0 degrees and theta=90 degrees was 0.41 and 0.28, respectively. Although the influence of tubule orientation was most important to mechanical behavior, the flexure strength and energy to fracture also decreased with an increase in tubule density. According to differences in the fatigue strength with tubule orientation, restorative practices promoting large cyclic normal stresses perpendicular to the tubules would be more likely to facilitate fatigue failure in dentin with cyclic loading.     

Transition behavior in fatigue of human dentin: structure and anisotropy

The influence of tubule orientation on the transition from fatigue to fatigue crack growth in human dentin was examined. Compact tension (CT) and rectangular beam specimens were prepared from the coronal dentin of molars with three unique tubule orientations (i.e., 0 degrees , 45 degrees and 90 degrees). The CT specimens (N=25) were used to characterize fatigue crack initiation and steady-state cyclic extension, whereas the rectangular beams (N=132) were subjected to 4-pt flexure and used in quantifying the stress-life fatigue response. The transition behavior was analyzed using both the Kitagawa-Takahashi and El Haddad approaches. Results showed that both the fatigue crack growth and stress-life responses were dependent on the tubule orientation. The average Paris Law exponent for crack growth perpendicular (90 degrees) to the tubules (m=13.3+/-1.1) was significantly greater (p<0.05) than that for crack growth oblique (45 degrees) to the tubules (m=11.5+/-1.87). Similarly, the fatigue strength of dentin with 90 degrees tubule orientation was significantly lower (p<0.05) than that for the other two orientations, regardless of the range of cyclic stress. The apparent endurance strengths of specimens with 0 degrees (44MPa) and 45 degrees (53MPa) orientations were nearly twice that of the 90 degrees (24MPa) orientation. Based on these results, human dentin exhibits the largest degree of anisotropy within the stress-life regime and the transition from fatigue to fatigue crack growth occurs under the lowest cyclic stress range when the tubules are aligned with the cyclic normal stress (90 degrees orientation).     

Cyclic fatigue-crack propagation, stress-corrosion, and fracture-toughness behavior in pyrolytic carbon-coated graphite for prosthetic heart valve applications

Fracture-mechanics tests were performed to characterize the cyclic fatigue, stress-corrosion cracking, and fracture-toughness behavior of a pyrolytic carbon-coated graphite composite material used in the manufacture of cardiac valve prostheses. Testing was carried out using compact tension C(T) samples containing "atomically" sharp precracks, both in room-temperature air and principally in a simulated physiological environment of 37 degrees C Ringer's lactate solution. Under sustained (monotonic) loads, the composite exhibited resistance-curve behavior, with a fracture toughness (KIc) between 1.1 and 1.9 MPa square root of m, and subcritical stress-corrosion crack velocities (da/dt) which were a function of the stress intensity K raised to the 74th power (over the range approximately 10(-9) to over 10(-5) m/s). More importantly, contrary to common perception, under cyclic loading conditions the composite was found to display true (cyclic) fatigue failure in both environments; fatigue-crack growth rates (da/dN) were seen to be a function of the 19th power of the stress-intensity range delta K (over the range approximately 10(-11) to over 10(-8) m/cycle). As subcritical crack velocities under cyclic loading were found to be many orders of magnitude faster than those measured under equivalent monotonic loads and to occur at typically 45% lower stress-intensity levels, cyclic fatigue in pyrolytic carbon-coated graphite is reasoned to be a vital consideration in the design and life-prediction procedures of prosthetic devices manufactured from this material.     

皮持骨在拉伸型,剪切型和撕裂型加载条件下的断裂韧性——纵向断裂…

对以质骨在拉伸、剪切和撕裂型载荷下的裂纹启裂韧性进行了研究。总数为１３０个紧凑拉式样,紧凑剪切试样和三腿型试样分别用于测量骨的拉伸型、剪切型和撕裂型启裂韧性。多试样柔度法用来测定当ａ／Ｗ＝０．５５（１,裂纹长度,Ｗ,试样宽度）时的临界能量释放率。临界应力强度因子由ａ／Ｗ＝０．５５的试样在试验中得到的临界载荷来计算。为了考察骨力学 各是性对于它的剪切型和撕裂裂纹启裂韧性的影响,对骨试样的裂纹扩展方向     

Hydration and dynamic fatigue of dentin

An experimental investigation on the dynamic fatigue response of dentin was conducted to examine the influence of stress rate on the strength and energy to fracture. Rectangular beams were prepared from the coronal dentin of bovine maxillary molars and subjected to four-point flexure to failure. The dentin beams were examined in the fully hydrated and dehydrated condition at stress rates (sigma) ranging from 0.01 to 100 MPa/s. Results for the hydrated dentin showed that the flexure strength, energy to fracture, and flexure modulus all increased with increasing stress rate; the flexure strength increased from 100 MPa ((sigma) = 0.01 MPa/s) to 250 MPa ((sigma) = 100 MPa/s). In contrast, the elastic modulus and strength of the dehydrated dentin decreased with increasing stress rate; the flexural strength of the dehydrated dentin deceased from 170 MPa ((sigma) = 0.01 MPa/s) to 100 MPa ((sigma) = 100 MPa/s). While the hydrated dentin behaved more like a brittle material at low stress rates, the strain to fracture was found to be nearly independent of (sigma). According to the experimental results, restorative conditions that cause development of static stresses within the tooth could promote a decrease in the damage tolerance of dentin.     

Fracture toughness, strength and slow crack growth in a ceria stabilized zirconia-alumina nanocomposite for medical applications

Mechanical properties and slow crack growth (SCG) behavior of a 10Ce-TZP/Al2O3 nanocomposite currently developed as a biomaterial are considered. Fracture toughness is determined for sharp, long (double torsion) and short (indentation) cracks and a good agreement is found between the two types of cracks. The main toughening mechanism in the nanocomposite is the tetragonal to monoclinic phase transformation of the ceria-stabilized zirconia (Ce-TZP) phase. Transformation at the surface of ground specimens leads to surface compressive induced stresses and an increase in strength. Crack velocity curves (V-K(I) curves) are obtained under static and cyclic fatigue using the double torsion method. The static V-K(I) curve in air reveals the three stages characteristic of stress corrosion with a threshold K(I0) approximately 4.5 MPa m(1/2) and a fracture toughness of 8.8 MPa m(1/2) significantly higher than those of currently used inert bioceramics (i.e., alumina and Y-TZP). A crack growth accelerating effect is shown under cyclic loading, correlated with a decrease in the threshold. However, the cyclic fatigue threshold (4 MPa m(1/2)) still stands above that of current biomedical grade alumina and zirconia.     

The suitability of different FEA models for studying root fractures caused by wedge effect

Finite element analysis (FEA) utilizing models with different levels of complexity are found in the literature to study the tendency to vertical root fracture caused by post intrusion ("wedge effect"). The objective of this investigation was to verify if some simplifications used in bi-dimensional FEA models are acceptable regarding the analysis of stresses caused by wedge effect. Three plane strain (PS) and two axisymmetric (Axi) models were studied. One PS model represented the apical third of the root entirely in dentin (PS-nG). The other models included gutta-percha in the apical third, and differed regarding dentin-post relationship: bonded (PS-B and Axi-B) or nonbonded (PS-nB and Axi-nB). Mesh discretization and material properties were similar for all cases. Maximum principal stress (sigma max) was analyzed as a response to a 165 N longitudinal load. Stress magnitude and orientation varied widely (PS-nG: 10.3 MPa; PS-B: 0.8 MPa; PS-nB: 10.4 MPa; Axi-B: 0.2 MPa; Axi-nB: 10.8 MPa). Axi-nB was the only model where all sigma max vectors at the apical third were perpendicular to the model plane. Therefore, it is adequate to demonstrate the tendency to vertical root fractures caused by wedge effect. Axi-B showed only part of the sigma max perpendicular to the model plane while PS models showed sigma max on the model plane. In these models, sigma max)orientation did not represent a situation where vertical root fracture would occur due to wedge effect. Adhesion between post and dentin significantly reduced sigma max.     

An examination of fatigue striations in human dentin: in vitro and in vivo

Although striations are often used in evaluating fatigue crack growth in engineering materials, they have not been used in studying the mechanics of fracture in hard tissues. The primary objective of this study was to evaluate the striations resulting from fatigue crack growth in the dentin of human teeth. Compact tension (CT) specimens obtained from the coronal dentin of molars from young (17 < or = age < or = 37 years) and senior (age > or = 50 years) patients were subjected to cyclic Mode I loads. Striations evident on the fracture surfaces were examined using a scanning electron microscope (SEM) and contact profilometer. Fatigue crack growth striations that developed in vivo were also examined on fracture surfaces of restored molars. A power spectrum analysis of surface profiles from the CT specimens showed that the striation spacing ranged from 50 to 170 microm. The average spacing in the dentin of seniors (130 +/- 23 microm) was significantly larger (p < 0.001) than that in young dentin (88 +/- 13 microm). Fatigue striations in the restored teeth exhibited features that were consistent with those that developed in vitro and a spacing ranging from 59 to 95 microm. Unlike metals, the striations in dentin developed after a period of cyclic loading that ranged from 1 x 10(3) to 1 x 10(5) cycles. A quantitative evaluation of the striation spacing using the Bates-Clark equation suggested that cyclic crack growth within the restored teeth occurred at a stress intensity range near 0.7 MPa x m(0.5), and a stress range of approximately 12 MPa.     

Effects of aging on the mechanical behavior of human dentin

An experimental study on the mechanical behavior of human dentin and the influence of age was conducted. Beams with rectangular cross-section were sectioned from the coronal dentin of virgin extracted molars (N = 76) that were obtained from (N = 70) patients between 17 and 80 years of age. The beams were loaded in either quasi-static 4-point flexure or 4-point flexural fatigue to failure and the stiffness, strength and fatigue properties were evaluated. In characterizing the fatigue response the beams were divided into two age groups that were regarded as young (17 < or = age < or = 30, mean +/- std. dev. = 25 +/- 5 years) and old (50 < or = age < or = 80, mean +/- std. dev. = 64 +/- 9 years) dentin. Results from monotonic loading showed that both the flexural strength and strain to fracture of dentin decreased significantly with age. The fatigue life of dentin increased with a reduction in cyclic stress amplitude and the fatigue strength of young dentin was greater than that of old dentin at all cyclic stress amplitudes. The endurance strength of young dentin (at 10(7) cycles) was approximately 44 MPa, whereas the old dentin exhibited an endurance strength of approximately 23 MPa.Based on differences in the mechanical behavior and microscopic features of the fracture surfaces from the young and old specimens, aging appears to result in an increase in both the rate of damage initiation and propagation in dentin.     

Relationship between fracture toughness and impact strength of acrylic bone cement

This work involved determining the fracture toughness, KIc (in MPa(square root)m) (using rectangular compact tension specimens) and impact strength, IS (in kJ/m2) (Charpy type specimens) of Surgical Simplex P and three variants of Palacos R acrylic bone cements. The best fit to these results yielded a power relationship KIc = 0.795(IS)0.59. The usefulness of this relationship is detailed, especially for the purpose of performing quality control checks on bone cements.     

Relative influence of composition and viscosity of acrylic bone cement on its apparent fracture toughness

The composition and viscosity of an acrylic bone cement have both been identified in the literature as being parameters that affect the mechanical properties of the material and, by extension, the in vivo longevity of cemented arthroplasties. The objective of the present study was to determine the relative influence of these parameters on a key cement mechanical property; namely, its fracture toughness. Two sets of cements were selected purposefully to allow the study objective to be achieved. Thus, one set comprised two cements with very similar compositions but very different viscosities (Cemex RX, a medium-viscosity brand, and Cemex Isoplastic, a high-viscosity brand) while the other set comprised two cements with similar viscosities but with many differences in composition (Cemex Isoplastic and CMW 1). Values of the fracture toughness (as determined using chevron-notched short rod specimens) [K(ISR)] obtained for Cemex RX and Cemex Isoplastic were 1.83 +/- 0.12 and 1.85 +/- 0.12 MPa square root(m), respectively, with the difference not being statistically significant. The K(ISR) values obtained for Cemex Isoplastic and CMW 1 were 1.85 +/- 0.12 and 1.64 +/- 0.18 MPa square root(m), respectively, with the difference being statistically significant. Thus, the influence of cement composition on its K(ISR) is more marked relative to the influence of cement viscosity. Explanations of this finding are offered, together with comments on the implications of the results for the in vivo longevity of cemented arthroplasties.     

Fatigue crack propagation rates in PMMA bone cement cannot be reduced to a single power law

Cement mantles around metallic implants have pre-existing flaws (shrinkage induced cracks, laminations, and endosteal surface features) and their fatigue failure is related to the fatigue crack propagation (FCP) rate of bone cement. We estimated the relevant in vivo range of cyclic stress intensity factor (DeltaK) around a generic femoral stem (0-1 MPa square root(m)) and determined that previous FCP data did not adequately cover this range of DeltaK. Vacuum-mixed standard bone cement was machined into ASTM E647 standard compact notched tension specimens. These were subject to sinusoidal loading (R = 0.1) at 5 Hz in 37 degrees C DI water, covering a DeltaK range of 0.25-1.5 MPa square root(m) (including a decreasing DeltaK protocol). FCP-rate data is normally reduced to a power-law fit relating crack growth rate (da/dn) to DeltaK. However, a substantial discontinuity was observed in our data at around DeltaK = 1, so two power-law fits were used. Over the physiologically plausible range of DeltaK, cracks grew at a rate of 2.9 E -8 x DeltaK(2.6) m/cycle. Our data indicated that FCP-rates for 0.5 > DeltaK > 0.3 MPa square root(m) are between 10 E -8 and 10 E -8 m/cycle, 1 or 2 orders of magnitude greater than predicted by extrapolating from previous models based on higher DeltaK data.     

A novel dentin bond strength measurement technique using a composite disk in diametral compression

New methods are needed that can predict the clinical failure of dental restorations that primarily rely on dentin bonding. Existing methods have shortcomings, e.g. severe deviation in the actual stress distribution from theory and a large standard deviation in the measured bond strength. We introduce here a novel test specimen by examining an endodontic model for dentin bonding. Specifically, we evaluated the feasibility of using the modified Brazilian disk test to measure the post-dentin interfacial bond strength. Four groups of resin composite disks which contained a slice of dentin with or without an intracanal post in the center were tested under diametral compression until fracture. Advanced nondestructive examination and imaging techniques in the form of acoustic emission (AE) and digital image correlation (DIC) were used innovatively to capture the fracture process in real time. DIC showed strain concentration first appearing at one of the lateral sides of the post-dentin interface. The appearance of the interfacial strain concentration also coincided with the first AE signal detected. Utilizing both the experimental data and finite-element analysis, the bond/tensile strengths were calculated to be: 11.2 MPa (fiber posts), 12.9 MPa (metal posts), 8.9 MPa (direct resin fillings) and 82.6 MPa for dentin. We have thus established the feasibility of using the composite disk in diametral compression to measure the bond strength between intracanal posts and dentin. The new method has the advantages of simpler specimen preparation, no premature failure, more consistent failure mode and smaller variations in the calculated bond strength.     

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%.     

Effect of orientation on the in vitro fracture toughness of dentin: the role of toughening mechanisms

Toughening mechanisms based on the presence of collagen fibrils have long been proposed for mineralized biological tissues like bone and dentin; however, no direct evidence for their precise role has ever been provided. Furthermore, although the anisotropy of mechanical properties of dentin with respect to orientation has been suggested in the literature, accurate measurements to support the effect of orientation on the fracture toughness of dentin are not available. To address these issues, the in vitro fracture toughness of dentin, extracted from elephant tusk, has been characterized using fatigue-precracked compact-tension specimens tested in Hank's balanced salt solution at ambient temperature, with fracture paths perpendicular and parallel to the tubule orientations (and orientations in between) specifically being evaluated. It was found that the fracture toughness was lower where cracking occurred in the plane of the collagen fibers, as compared to crack paths perpendicular to the fibers. The origins of this effect on the toughness of dentin are discussed primarily in terms of the salient toughening mechanisms active in this material; specifically, the role of crack bridging, both from uncracked ligaments and by individual collagen fibrils, is considered. Estimates for the contributions from each of these mechanisms are provided from theoretical models available in the literature.     

Age, dehydration and fatigue crack growth in dentin

A preliminary study of the effects from age and dehydration on fatigue crack growth in human dentin was conducted. Compact tension (CT) fatigue specimens of coronal dentin were prepared from extracted molars and subjected to high cycle fatigue (10(5)相似文献