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Biomaterials 24 (2003) 3955--3968 Effect of orientation on the in vitro fracture toughnes of dentin: the role of toughening mechanisg

Biomaterials 24 (2003) 3955--3968 Effect of orientation on the in vitro fracture toughnes of dentin: the role of toughening mechanisg
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  Biomaterials 24 (2003) 3955–3968 Effect of orientation on the in vitro fracture toughness of dentin:the role of toughening mechanisms $ R.K. Nalla a , J.H. Kinney b , R.O. Ritchie a, * a Materials Sciences Division, Lawrence Berkeley National Laboratory, Department of Materials Science and Engineering,University of California, Berkeley, CA 94720, USA b Department of Preventive and Restorative Dental Sciences, University of California, San Francisco, CA 94143, USA Received 3 December 2002; accepted 8 April 2003 Abstract Toughening mechanisms based on the presence of collagen fibrils have long been proposed for mineralized biological tissues likebone 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 supportthe effect of orientation on the fracture toughness of dentin are not available. To address these issues, the in vitro fracture toughnessof dentin, extracted from elephant tusk, has been characterized using fatigue-precracked compact-tension specimens tested inHank’s balanced salt solution at ambient temperature, with fracture paths perpendicular and parallel to the tubule orientations (andorientations in between) specifically being evaluated. It was found that the fracture toughness was lower where cracking occurred inthe plane of the collagen fibers, as compared to crack paths perpendicular to the fibers. The srcins 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 crackbridging, both from uncracked ligaments and by individual collagen fibrils, is considered. Estimates for the contributions from eachof these mechanisms are provided from theoretical models available in the literature. r 2003 Elsevier Science Ltd. All rights reserved. Keywords:  Collagen; Fracture toughness; Tubules; Orientation; Toughening mechanisms; Dentin 1. Introduction Dentin is the most abundant mineralized tissue in thetooth. Similar in composition to bone, it is composedlargely of type-I collagen fibrils and nanocrystallineapatite mineral [1]. The most striking microstructural feature is the dentinal tubule, cylindrical channels thatcourse continuously from the dentin–enamel andcementum–enamel junctions to the pulp. A thin, highlymineralized cuff of peritubular dentin surrounds eachtubule. The mineralized collagen fibrils are arrangedorthogonal to the tubules, forming a planar, felt-likestructure called the intertubular dentin matrix [2]. Thishighly oriented microstructure is believed to conferanisotropy to the mechanical properties, although themagnitude and orientation of the anisotropy is not wellestablished. Indeed, after some five decades of researchon the mechanical properties of dentin (e.g., [3–15]),there is still little consistency in some of the basicquestions that dictate its structural behavior.Because the peritubular dentin is highly mineralized,it had long been suspected that dentin had a higherelastic modulus in the direction of the tubules. However,recent micromechanics arguments [12] and sensitiveacoustic measurements [3] now support the view that theelastic properties are determined by the mineralizedcollagen fibers, and that dentin is therefore stiffest in anorientation perpendicular to the axes of the tubules.These more recent results have largely substantiated forhuman dentin what had been observed in an earlierstudy on Narwhal tusk dentin by Currey et al., namely,that there is a strong dependence of the elastic propertieson the orientation of the mineralized collagen fibrils [15].The observations that the orientation of the collagenfibrils affects the symmetry of the elastic propertiessuggest that their orientation might also influence ARTICLE IN PRESS $ This work was supported in part by the National Institutes of Health, National Institute for Dental and Craniofacial Research underGrant No. P01DE09859.*Corresponding author. Tel.: +1-510-486-5798; fax: +1-510-486-4881. E-mail address: (R.O. Ritchie).0142-9612/03/$-see front matter r 2003 Elsevier Science Ltd. All rights reserved.doi:10.1016/S0142-9612(03)00278-3  fracture behavior. This is important as resistance tofracture in teeth is an issue of great clinical relevance.Exposed root surfaces often exhibit non-carious notchesin the dentin just below the enamel–cementum junction,which can act as sites for unstable fracture. While cuspfractures are common in posterior teeth, the anteriorteeth are more susceptible to fracture in the gingiva,severing the crown of the tooth. Although such fractureshave not been investigated extensively, it is generallybelieved that they are catastrophic events induced byocclusal stresses. In light of this, some measure of thefracture resistance of dentin is necessary.Fracture mechanics provides an appropriate metho-dology to quantify the fracture resistance of dentin.Under linear-elastic conditions, fracture instability isreached when the stress intensity ahead of a pre-existingcrack exceeds the fracture toughness,  K  c , of the material,i.e., K   ¼  Y  s app ð p a Þ 1 = 2 ¼  K  c ;  ð 1 Þ where  s app  is the applied (service) stress,  a  is the cracklength, and  Y   is a function of geometry, crack size andshape (and of order unity). Alternatively, the fracturetoughness can be expressed in terms of a critical value of the strain energy release rate,  G  c ;  defined as the changein potential energy per unit increase in crack area, where G  c  ¼  K  2c  = E  0 ;  ð 2 Þ and where  E  0 ¼  E  ;  the elastic modulus in plane stressand  E  = ð 1    n 2 Þ  in plane strain ( n  is Poisson’s ratio) [16].To date, only a few studies have provided aquantitative evaluation of the fracture toughness of dentin. The earliest was by Rasmussen et al. [8,9] whoused a ‘‘work of fracture’’ (defined as the work per unitarea to generate new crack surface) to quantify thefracture resistance. These authors reported an orienta-tion effect on the toughness of dentin in that the work of fracture was found to be lower for cracking perpendi-cular to the dentinal tubular direction, i.e., in the planeof the mineralized collagen fibrils, compared to all otherdirections. Such a result is consistent with the notionthat crack bridging by the collagen fibrils could enhancethe toughness along directions parallel to the tubuleaxes. Indeed, Ref. [8] does indicate that crack propaga-tion perpendicular to the tubules is more energeticallyfavorable, consistent with the absence of fiber bridgingin that direction. However, excessive scatter in theirresults makes such definitive conclusions difficult;moreover, no direct evidence of such bridging waspresented.A subsequent study, by el Mowafy et al. [10], was the first to utilize a fracture mechanics approach, usingnotched (but not precracked) compact-tension speci-mens to measure the fracture toughness of humandentin to be  K  c  ¼  3 : 08MPa O m (SD 0.33MPa O m) for asingle orientation parallel to the long axis of the tubules.In a similar vein, Iwamoto et al. [13] reported fracturetoughness values for human dentin (1.13 7 0.36MPa O mto 2.02 7 0.18MPa O m, depending on orientation), usingthe so-called notchless triangular prism specimengeometry. The latter technique permits the use of verysmall samples, which allowed these authors to also showan effect of orientation on toughness; however, theaccuracy of their  K  c  data may be deemed to besomewhat questionable in light of the non-standardnature of their toughness tests. Most recently, Imbeniet al. [14] used fatigue-precracked three-point bend barsamples (nominally conforming to ASTM standards) inorder to determine an accurate measure of the in vitrofracture toughness of human dentin. 1 Measurements,made for a crack path perpendicular to the tubules inorder to determine a worst-case value, yielded a fracturetoughness of   K  c  ¼  1 : 79MPa O m (SD 0.1). Due tospecimen size requirements, other orientations couldnot be examined.These limited results suggest that the fractureresistance of dentin is anisotropic, although an accuratequantification of the variation in  K  c  with orientation isstill lacking and the precise mechanisms underlying theeffect are as yet unproven. Part of the problem has beenthe relatively small size of the specimens that can bemade with human dentin, which makes it difficult toaccurately address the role of orientation on toughness.To alleviate this problem in the present work, we havechosen to study elephant dentin, which permits the useof specimens of appropriate size to determine validmeasurements of the fracture toughness in all relevanttubule, and hence collagen, orientations. Specifically, weaddress several critical hypotheses in a systematicevaluation of effect of orientation on the fracturetoughness and of the crack-microstructure interactionsin elephant dentin: * What is the role of collagen fibril orientation on thetoughness? * Does fibril bridging occur in a mineralized tissue of composition similar to bone? * Is the anisotropy of the fracture toughness consistentwith such crack bridging? * Do the tubules affect the toughness, either byblunting or deflecting cracks? * Are there other salient mechanisms of toughening indentin?It is believed that some resolution of these issuesprovides insight into the functional role of microstruc-ture, and specifically the collagen fibrils, in influencingthe fracture of mineralized tissue. ARTICLE IN PRESS 1 These authors demonstrated a marked effect of notch acuity on thetoughness values, thereby indicating that earlier measurements of thefracture toughness of dentin, which used notched rather thanprecracked samples (e.g., [10]), gave unrealistically high values. R.K. Nalla et al. / Biomaterials 24 (2003) 3955–3968 3956  2. Materials and experimental procedures  2.1. Materials Recently fractured shards of elephant tusk from anadult male elephant ( Loxodonta africana ) were used inthe present study. The bulk of the tusk material, which iscommonly referred to as ivory, is composed of dentin. Atypical scanning electron micrograph of the microstruc-ture of the material used is given in Fig. 1a, showing anorientation perpendicular to the long axis of the dentinaltubules. Akin to human dentin, the characteristic featureof this microstructure is the presence of tubules that arethe result of odontoblast cell movement during dentinformation. These tubules sit in a matrix formed by themineralization of type I collagen fibers deposited in theearly stages of formation [17]. At this juncture, it isimportant to point out that although the microstructureis very similar to that of human dentin, there are someessential differences: the tubules are more elliptical inshape [17] and the peritubular cuff is comparatively verysmall or nonexistent (Fig. 1b). In vitro tensile yield ( s y )and ultimate tensile ( s UTS ) strengths levels weremeasured in Hank’s balanced salt solution (HBSS) tobe  s y B 50 2 65MPa and  s UTS B 70 2 80MPa, respec-tively. Elastic moduli were obtained from sound speedmeasurements made along orientations perpendicularand parallel to the tubule axis; values of   B 13–17GPafor the Young’s modulus, 5–6GPa for the shearmodulus were obtained, with the higher values asso-ciated along the directions perpendicular to the tubules[18].  2.2. Fracture toughness tests Five different orientations were examined, as shownschematically in Fig. 2, with a total of   N   ¼  16 testsamples: * Tubule long axis perpendicular to the notch plane( XZ  ) and notch direction ( Y  ) referred to as ‘‘perpen-dicular’’ orientation (Fig. 2a)—( N   ¼  3), * Tubule long axis inclined (nominally at B 45  ) to thenotch plane and notch direction referred to as‘‘inclined perpendicular’’ orientation (Fig. 2b)— ( N   ¼  3), * Tubule long axis parallel to the notch plane andnotch direction, referred to as ‘‘in-plane parallel’’orientation (Fig. 2c)—( N   ¼  3), * Tubule long axis parallel to the notch plane andperpendicular to notch direction, referred to as ‘‘anti-plane parallel’’ orientation (Fig. 2d)—( N   ¼  3), and * Tubule long axis parallel to the notch plane andinclined (nominally at B 45  ) to the notch direction,referred to as ‘‘inclined parallel’’ orientation(Fig. 2e)—( N   ¼  3).It should be noted here that the orientation can bedifficult to define in advance as the tubules often do nottake a straight path, as illustrated in Fig. 3 by the curvedpath of the tubules on a fracture surface for one of the‘‘in-plane parallel’’ orientations. Similar observationshave previously been reported for both human [4] andelephant dentin [17]. In fact, with the exception of theroot, the tubules in human dentin do not run a straightcourse from the enamel to the pulp; rather, from thecervical margin through the crown, the tubules have acomplex, S-shaped curvature [19]. In light of this, it isalmost impossible to align the fracture plane preciselywith the tubule axes a priori, and post-fractographicobservations must be used to determine the exactorientation.For each orientation, fracture toughness tests wereperformed in general accordance with ASTM Standards[20]. Compact-tension, C(T), samples (Fig. 4) were used, ARTICLE IN PRESS Fig. 1. (a) Scanning electron micrographs of the typical microstructureof elephant tusk dentin used in this study (in the plane perpendicularto the long axis of the tubules). The inset shows a schematic of the orientation of the collagen fibrils with respect to the tubules.(b) Scanning electron micrographs of a tubule. Note in comparison tohuman dentin, the slightly elliptical shape of the tubule and the lack of a mineralized peritubular dentin cuff. R.K. Nalla et al. / Biomaterials 24 (2003) 3955–3968  3957  and were machined from 15-mm 3 cubes of dentin, whichwere first obtained through rough sectioning. Aftermachining, specimens were wet polished up to a 1200-grit finish, followed by a final polishing step using a 1 m malumina suspension. Specimens with widths of   W  B 3 : 5– 7mm and thicknesses of   B  B 0 : 75–1.25mm were used 2 (Fig. 4). The initial portion of the notch was carefullymachined using a slow speed saw, with the final portionbeing introduced using a fine blade; this yielded notchroot radii of typically  r B 10–20 m m. Samples were thenfatigue precracked in room air at a nominal stress-intensity range of   B 0.9MPa O m to a crack length towidth ratio of   a = W  B 0 : 45 2 0 : 55 : The C(T) specimens were loaded to failure in vitro inHBSS at ambient temperature using an ELF s 3200series voice coil-based mechanical testing machine(EnduraTEC Inc., Minnetonka, MN). The tests wereperformed under displacement control with a constantcross-head movement rate of 0.02mm/min. In accor-dance with the ASTM Standard E-399 for Plane-StrainFracture Toughness testing [20], the fracture toughness, K  c  at fracture was calculated from the load history usingthe expression: K  c  ¼  P  c BW  1 = 2  f  ð a = W  Þ ;  ð 3 Þ where  P  c  is the load at fracture instability,  B   is thespecimen thickness,  W   is the specimen width,  a  is thenotch plus crack length, and  f  ð a = W  Þ  is dimensionlessfunction of   a = W   given by  f  ð a = W  Þ ¼ ½ 2  þ ð a = W  Þ½ 0 : 866  þ  4 : 64 ð a = W  Þ   13 : 32 ð a = W  Þ 2 þ  14 : 72 ð a = W  Þ 3   5 : 6 ð a = W  Þ 4 ½ 1   ð a = W  Þ 3 = 2  : ð 4 Þ According to ASTM Standard E-399, a state of planestrain is achieved when the sample thickness is greaterthan 2 : 5 ð K  c = s y Þ 2 ;  i.e., the thickness is significantly largerthan the plastic or damage zone size of  r y B 1 = 2 p ð K  c = s y Þ 2 :  For elephant dentin, this wouldrequire samples thicknesses greater than approximately1–3mm to yield a plane-strain  K  c  value. However, asthis criterion is generally quite conservative and thedamage zone was well contained within the specimen ARTICLE IN PRESS (a) Perpendicular  (b) Inclined Perpendicular  (c) In-plane Parallel  (d) Anti-plane Parallel  (e) Inclined Parallel XYZ nominal crack propagation direction tubules Fig. 2. Schematics of the five orientations used in this investigation. The reference coordinate system with the crack in the  XZ   plane and the directionof nominal crack propagation in the  X   direction are also shown. 50 µ m crack growth direction Fig. 3. A scanning electron micrograph of a fracture surface obtainedfor a ‘‘parallel’’ orientation specimen. Clearly, the tubules do not runin a straight course, but take a rather complex curved path. Thedirection of nominal crack growth is shown. 2 It should be noted that little variation in toughness was found in agiven orientation over this range of thicknesses, consistent withconditions approaching that of plane strain (see below). R.K. Nalla et al. / Biomaterials 24 (2003) 3955–3968 3958  boundaries, it is believed that the toughness valuesmeasured with the current test specimens would be veryclose to this lower bound.  2.3. Fractographic observations Post-failure fractographic observation of the fracturesurfaces of the failed C(T) specimens were made in thescanning electron microscope (SEM), operating at 6– 10kV in a conventional back-scattered electron mode.Samples were imaged after first coating with a gold– palladium alloy. In addition to providing informationon the mechanisms of fracture, these observations werenecessary to determine unambiguously the orientationof the fracture plane with respect to the tubules.  2.4. Crack path observations To understand the mechanisms associated with howmicrostructural orientation affects fracture in dentin,crack path trajectories were examined. However, sincefracture in dentin tends to be brittle in nature, withcrack initiation essentially simultaneous with unstable(catastrophic) fracture, a novel double-notch four-pointbend geometry was used to generate a stable crack(Fig. 5). This technique, which has been previously usedby the authors to discern whether fracture is locallystress- or strain-controlled in human dentin [4], involvesloading a beam with two nominally identical notches tofailure under four-point bending. Under four-point(pure) bending, both notches experience the samebending moment; thus when one notch fails, themicrostructure and local cracking events immediatelyprior to unstable fracture are effectively ‘‘frozen-in’’ atthe unfractured notch. Since in the presence of somedegree of inelastic deformation (e.g., plastic deforma-tion), the maximum local  strains  are  at  the notch rootwhereas the maximum local  stresses  are  ahead   of thenotch (near the elastic/plastic interface), the location of the local cracking events prior to instability gives an ARTICLE IN PRESS (a) (b) 1 mm XY Z Nominal Crack Propagation Direction a W  B Fig. 4. (a) A schematic illustration of the compact-tension specimen geometry used in the present study. Typically,  a = W   ratios of  B 0.45–0.55 wereutilized. Also shown is the reference coordinate axis system used for describing the orientation of the specimens. (b) An optical photomicrograph of atypical specimen is given. R.K. Nalla et al. / Biomaterials 24 (2003) 3955–3968  3959
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