AN APPLICATION OF MICROSCOPIC DIGITAL IMAGE CORRELATION TO DENTAL MATERIALS Dwayne Arola, Ahmad Nazari Department of Mechanical Engineering, University of Maryland Baltimore County, Baltimore, MD 21250 darola@umbc.edu anazari1@umbc.edu Miao Luo, ♣Dongsheng Zhang Department of Mechanics, Shanghai University, Shanghai, 200444, PR China luomiao82@hotmail.com donzhang@staff.shu.edu.cn ABSTRACT An understanding of the fatigue and fracture behavior of dental materials is critical to the maintenance of physical and oral health. Recent studies suggest that there are a number of mechanisms contributing to crack extension and crack arrest in these materials, and that they appear to be a function of moisture and age of the tissue. An understanding of these processes can provide new ideas that are relevant to the design of multi-functional engineering materials. As a result, we have adopted the use of microscopic Digital Image Correlation (DIC) to examine the mechanisms of crack growth resistance and near-tip displacement distribution for cracks in human dentin that are subjected to opening mode loads. In this paper we describe application of these experimental methods and present some recent results concerning fatigue crack growth and stable crack extension in dentin. Introduction The mechanical properties of the human tooth have been of interest for many decades. While the strength and elastic modulus of these tissues have been examined in detail, comparatively few studies have evaluated their fatigue and fracture behavior [1]. An understanding of crack initiation and growth in hard tissues of the human body is essential for the successful development of medical and dental treatments aimed at maintaining a high quality of life [2,3]. While there are many existing questions, studies conducted over the past decade have provided a foundation for further understanding. Recent investigations of dentin indicate that the fracture toughness ranges from 1 to 2 MPa•m0.5 [4,5] and that the lowest toughness is exhibited for cracks extending perpendicular to the dentin tubules. Dentin exhibits an increase in toughness with crack extension, which is at least partially attributed to bridging forces resulting from collagen fibrils and ligaments of dentin tissue spanning the crack [6,7]. Energy dissipation is also believed to occur through inelastic deformation adjacent to the crack tip, a process that is not currently well understood [8]. Tubule orientation and hydration have been shown to play an important role on the crack growth resistance of dentin through differences in the contribution of toughening mechanisms. While fracture is a relevant concern, the initiation and growth of cracks due to fatigue are potentially of greater importance. Studies on fatigue crack growth in human dentin [6,7] have shown that cyclic crack growth can be modeled using the Paris Law 0.5 and occurs over a stress intensity range from approximately 0.7 to 2 MPa•m . Complementary studies in this area have shown that the rate of crack growth is dependent on the tubule orientation [8], increases with mean stress [9] and increases with a reduction in loading frequency [10]. Also, recent results have shown that structural changes that occur in dentin with aging appear to contribute to a reduction in the resistance to crack initiation [11] and facilitate an increase in the fatigue crack growth rate [7]. Paris law exponents for cyclic crack growth reportedly range between 8 and 13 for the dentin of comparatively young patients (18≤age≤35), whereas the value increases to over 20 for dentin of more senior patients (age≥50). In this paper we describe some novel experimental techniques that have been adopted/developed for examining the fatigue and fracture behavior of hard tissues. The overall objectives of the manuscript are to present the methodology, validate their application, and to convey their value in studying fracture processes in hard tissues, particularly in instances where the size of tissue available is limited and standardized methods are not sufficient. The methods of evaluation are described in detail and ♣ Corrsponding Author representative results are presented and discussed. Materials and methods In the following studies the dentin of human teeth were examined. To support these efforts, second and third molars were acquired from participating dental practices in Maryland according to an approved protocol by the Institutional Review Board of the University of Maryland Baltimore County. All teeth were stored immediately after extraction in a bath of Hanks Balanced Salt Solution (HBSS) at 2°C, and maintained in hydration during all aspects of specimen preparation. Overall, the experimental methods used in evaluating these tissues were comprised of developing specimens of selected tissue and application of an optical approach for both characterizing and quantifying crack extension. In addition, microscopic digital image correlation was adopted to evaluate the mechanics of fracture and identify mechanisms contributing to crack growth resistance. Specimen Preparation The experimental evaluation was conducted using CT specimens. A CT specimen comprised completely of dentin (Fig. 1) can generally be obtained from the crown of an unrestored molar. In the present study, sections of dentin were obtained from the crown using diamond impregnated slicing equipment and continuous hydration. The methods and equipment used for sectioning have been described in detail elsewhere [8]. B* 1 4 a W 2 B 6 Figure 1 schematic diagram of the “standard” dentin CT specimen The dentin CT specimens were gently sanded on both sides using #220 mesh SiC paper to obtain a uniform cross-section. A channel was also introduced on the back of all specimens to guide the direction of crack extension using diamond impregnated slicing wheels (of #320 mesh particles) and a programmable slicer/grinder. Two holes were drilled for application of the opening mode loads (Fig. 1) and counter-bored to a depth equivalent to that of the channel. Counter-boring insured that the resolved opening loads were located centrally about the reduced specimen thickness (B*) adjacent to the channel. Lastly, a notch was machined (Fig. 1) using a diamond impregnated slicing wheel and the tip was sharpened using a razor blade and diamond paste (1 or 8 µm particles) to facilitate crack initiation. Equipment and Procedures The CT specimens were subjected to either quasi-static or cyclic Mode I loads for different aspects of evaluation. All specimens were subjected to cyclic loading at first to initiate a crack from the sharpened notch. Cyclic loading was performed using an Enduratec Model 3200 universal testing system with the specimens immersed in a hydration bath (22°C). Crack initiation was achieved using a stress ratio (R) of 0.5 and frequency of 5 Hz with maximum load of approximately 5 Newtons. Cyclic loading of the specimens was continued using R=0.1, with maximum load of between 8 to 12 Newtons, until the crack was extended a length of approximately 0.5 mm past the notch. The extension was used to reduce notch effects during further cyclic or quasi-static loading. The dentin and inset CT specimens was performed using a specially designed universal testing system, complemented with microscopic imaging equipment comprised of a specially designed miniature universal loading frame, a stereomicroscope and a control computer (Fig. 2). The loading frame is fully automated, enables load or displacement control actuation and has a load range of 100 Newtons with precision of 0.05%. In addition, the system utilizes a central lead screw with both left- and right-hand lead, which results in simultaneous actuation of both grips in opposite directions. As a result, the system minimizes changes in the field of view that are typical with single lead systems. The microscopic imaging system consists of a stereo light microscope (Nikon SMZ-1000) with optical output for a camera, a progressive scan CCD camera (JAI CV-A1 CCD camera) and an imaging board. With a fixed zoom ratio of 10:1, a 1X objective lens and a 1X step-up ring at the output of the microscope, the optical system allows up to 200X magnification using the aforementioned camera and microscope. A single computer is used with dedicated software to control the load frame, sample the load and displacement data, as well as acquire and synchronize the digital images with the load/displacement response. The load, load-line displacement responses and crack length measurements were used with results of a numerical model for estimating the apparent toughness. Figure 2 Experimental arrangement The microscopic system was adjusted to capture images from the specimen’s surface over a field of view of approximately 3x4 mm, with a resolution of 1376X1035 pixels and in grayscale mode. Opening mode loads were applied in increments of 0.5 to 1 Newton, until the onset of cracking was identified from reduction in the apparent stiffness. Loading was then continued in displacement control in increments of approximately 0.5 Newton and lower, followed by a dwell at each load increment (typically of 2 min), and then followed by partial unloading and reloading. The dwell-time was utilized to examine time-dependent changes in crack extension under constant load line displacement. Digital images were acquired at the onset of loading, at the peak load, and after the dwell time to document the crack growth process. These procedures were followed through progressive increments of crack extension until the onset of instability. Images of a glass plate with precision cross-grating and fixed spatial frequency were acquired after the experiment and used to convert the documented field of view into physical dimensions and to correct for potential errors caused by lens aberration [12]. Micro Digital Image Correlation Digital image correlation has found a tremendous number of applications in quantifying displacement and strain distributions within the field of experimental mechanics [13]. Despite some difficulties, applications within the field of biomechanics are becoming more common [e.g. 14-17]. In the present study, DIC was employed to quantify the full-field displacement distribution that resulted from crack extension. Briefly, digital images of the specimen’s surface in the plane of loading were acquired at an initial (before loading) and deformed condition (under load). The displacement at each location within the field of view was determined from a correlation of the grayscale distribution of the deformed and reference images. A cross correlation algorithm was employed to compare subsets of the images according to (1) < F1 ⋅ F2 > − < F1 > ⋅ < F2 > C= 1 [< ( F1 − < F1 > ) 2 > ⋅ < ( F2 − < F2 >) 2 >] 2 where F1 and F2 are grayscale matrices of subsets of pixels in the initial and deformed images, respectively. The symbol <> in Eqn. (1) represents the mean value of the elements in the matrix. Lens aberration can cause distortion between the image plane and the object plane. As the main distortions are radial and perspective related, the lens distortion distribution of light microscopes can be presented as the warping function having first-order and second-order terms, defined as follows, ⎧⎪δ x ( xi , yi ) = a0 + a1 xi + a 2 yi + a3 xi 2 + a 4 xi yi + a5 yi 2 + a6 xi 3 + a7 xi 2 yi + a8 xi yi 2 + a9 yi 3 ⎨ 2 2 3 2 2 3 ⎪⎩ δ y ( xi , yi ) = b0 + b1 xi + b2 yi + b3 xi + b4 xi yi + b5 yi + b6 xi + b7 xi yi + b8 xi yi + b9 yi where (2) xi and yi are coordinate locations in the image plane, and ai and bi (i = 0L9) are coefficients to be determined. Aberration errors ( δ x and δ y ) in this paper were assessed by using a precise cross-grating plate with fixed spatial frequency as a standard. Images of the grating were acquired with the same microscopic imaging system. Two independent equations represented the aberration distributions are generated according to eqn. 2 by all of the cross-grating nodes[12]. Numerical Methods According to the unique geometry of the dentin CT specimens (Fig. 1), the stress intensity distribution with crack growth could not be estimated using relationships provided by ASTM standards E399 [37] or E647 [38]. The stress intensity distribution was evaluated across the specimen thickness, and as a function of the crack length. The distribution in KI with crack extension for the standard CT specimens as described in Figure 1(a) is given by 1 ⎛ B* +1 ⎞ 2 KI = ⎜ ⎟ (0.131 + 0.320α + 0.211α 2 ) [MPa•m0.5] B* W ⎝ B+1 ⎠ P (1.4≤a≤3.0) (3) where P is the opening load (in Newtons), is the ratio of a to W (Fig. 1) and the quantities B* and B are the ligament thickness (within the region of the channel) and nominal specimen thickness, respectively. All parameters of geometry in Eqn. 3 are to be introduced in millimeters. RESULTS The opening mode load was applied in displacement control to achieve stable crack extension from the fatigue crack. Incremental loading of the specimens was then continued to achieve sub-critical crack growth until reaching a critical length. A representative image of the full field opening mode displacement (v) associated with crack growth is shown in Figure 3(a). Displacement distributions were determined from digital images taken after each increment of crack extension. These were used to identify the incremental crack tip location, as evident from the v-distribution (where v=0), and in determining the COD distribution. Typical COD profiles are shown in Figure 3(b) that were obtained immediately following crack arrest (time=0 min), and after a 2 minute dwell from crack extension (time=2 min), in which the load-line displacement was held constant. 10 COD/2 (µm) 8 6 4 2 0 0.0 time = 0 min time = 2 min 0.2 0.4 0.6 0.8 1.0 1.2 Distance from Crack tip (mm) (a) displacement field near the crack tip (b) COD profile at crack tip Figure 3 Analysis of the mechanics of fracture associated with crack extension in human dentin The load history and crack length measurements were used in evaluating the crack growth resistance of human dentin with crack extension (∆a). Two specimens were obtained from a young (age=18) and more senior (age=55) patient. To aid in characterization, the initiation toughness (Ko) has been defined at the inception of crack extension, a growth toughness (Kg) used to quantify the increase in toughness with crack extension, and a critical stress intensity (i.e. fracture toughness; Kc) defined at either the plateau or maximum toughness. The Ko for the young and old specimen is 1.2 and 1.1 MPa•m0.5, respectively, and the growth toughness for both specimens is approximately 1.1 MPa•m0.5/mm. The Kc for the young dentin was found to be 1.65 MPa•m0.5, in comparison to 1.30 MPa•m0.5 for that of the senior patient (more than 20% lower). Both responses show rising toughness with crack extension. The toughening in these responses is commonly observed and expected to at least partially result from the development of ligaments that are regularly identified behind the crack. DISCUSSION Through application of DIC, the opening mode displacement distribution was obtained about the crack tip during stable crack extension in CT specimens of human dentin. Using these distributions, representative COD profiles were presented for stable cracks immediately after extension, and after a 2 minute period of relaxation under constant load-line displacement. While optical observations of crack-tip blunting have been reported for crack growth in hydrated elephant dentin [10], the contribution of this mechanism to crack growth resistance in human dentin has not been previously reported. One benefit of adopting microscopic DIC for studying the fracture process in hard tissues is the ability to observe and quantify the near tip mechanics that contribute to the apparent toughness. Mechanisms potentially contributing to the non-linearity and time dependence include the movement of bound water and hydraulic processes, microcracking adjacent to the crack tip, and/or the non-linear extension of the collagen fibrils. Further research is underway to identify the specific mechanisms responsible and the significance of their contribution to crack arrest. There are many obstacles to evaluating the fatigue and fracture properties of hard tissues and obtaining reliable results. Firstly, the standardized methods of characterization cannot often be applied due to the restricted volume of tissue available. Some would argue that indentation fracture provides an alternative to the techniques presented, and eliminates the size constraints. However, a recent review has addressed the shortcomings of indentation fracture tests, particularly in regards to the load dependence [19]. Toughness estimates from indentation fracture may be 50 to 100 % in error. The need to maintain hydration of the tissue and inherent moisture poses further difficulties, particularly with application of optical methods for documenting the fracture process. Interferometric methods, which have been commonly employed for quantifying fracture processes in engineering materials, are not as robust when applied to moist substrates. Yet, an optical examination of the fracture process is invaluable in this area due to the opportunity for identifying important mechanisms contributing to the quantitative measurements. Post-process evaluations of the fracture surfaces (using fractography) can be of equal value in examining fracture in hard tissues [20]. Through microscopic digital imaging and use of DIC, both qualitative and quantitative information can be obtained with a displacement resolution that fully supports the comparatively large range in displacements associated with fracture in hydrated hard tissues. By combining the benefits of microscopic DIC with unique approaches for preparing and loading specimens, a detailed and reliable understanding of fatigue and fracture within hard tissues is possible. It is hoped that the techniques described herein will enable many future studies of hard tissues that are otherwise considered impossible. SUMMARY Some novel experimental approaches were presented for examining the mechanisms of crack growth resistance and near-tip displacement distribution associated with sub-critical crack growth in hard tissues. Successful application of microscopic DIC in examination of crack growth in dentin of human teeth shows that it is a suitable non-contact optical method for evaluating the mechanics of fracture in hard tissues. New results on the crack opening displacement (COD) distribution of human dentin were obtained. While applications were limited to the human tooth, the methods introduced in this study would serve equally well for examining crack extension in other hydrated tissue or for material systems where there are geometric constraints. The methods should support future studies aimed at development of new knowledge on the mechanics of fatigue and fracture in selected hard tissues. ACKNOWLEDGEMENT This research was supported in part by the National Science Foundation (BES 0238237) and the American Association of Endodontists Foundation. The author A. Nazari also wishes to acknowledge support from a GAANN Fellowship. The authors would also thank the support of the National Science Foundation of China under Grand # 30672348 and Shanghai Pujiang program. REFERENCES Kinney JH, Marshall SJ, Marshall GW. The mechanical properties of human dentin: a critical review and re-evaluation of the dental literature. Crit Rev Oral Biol Med. 2003;14:13-29. 2. 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