Search

Osteoporosis, which is correlated with low bone mass and increased bone fragility, is responsible for about 1.2 million fractures per year in the United States. We have used the three-dimensional (3-D), X-ray tomographic microscope to image the trabecular bone architecture of the proximal tibias of six Sprague-Dawley rats in vivo. Three of these rats were then ovariectomized to induce estrogen depletion, and three remained as controls. Five weeks later, the tibias were reimaged. The ovariectomized rats lost approximately 65% of their trabecular bone volume as compared with an insignificant change in the control rats. The connectivity density of the trabecular bone, as measured by the Euler characteristic, was linearly correlated with trabecular bone volume, even in the ovariectomized rats. Hypoestrogenemic bone loss manifested itself in greatly reduced connectivity and fewer trabecular elements, but not in thinning of trabeculae. The ability to microscopically image sequential changes in the 3-D architecture of trabecular bone in vivo will allow exploration of the earliest stages of hypoestrogenemic bone loss and to more rapidly test the effectiveness of new clinical treatments for this major public health problem.

Hot-spot models of initiation and detonation show that voids or porosity ranging from nanometer to micrometer in size within highly insensitive energetic materials affect initiability and detonation properties. Thus, the knowledge of the void size distribution, and how it changes with the volume expansion seen with temperature cycling, are important to understanding the properties of the insensitive explosive 1,3,5-triamino-2,4,6-trinitrobenzene (TATB). In this paper, void size distributions in the 2 nm to 2 μm regime, obtained from small-angle X-ray scattering measurements, are presented for LX-17-1, PBX-9502, and ultra-fine TATB formulations, both as processed and after thermal cycling. Two peaks were observed in the void size distribution: a narrow peak between 7–10 nm and a broad peak between 20 nm and about 1 mm. The first peak was attributed to porosity intrinsic to the TATB crystallites. The larger pores were believed to be intercrystalline, a result of incomplete consolidation during processing and pressing. After thermal cycling, these specimens showed an increase in both the number and size of these larger pores. These results illuminate the nature of the void distributions in these TATB-based explosives from 2 nm to 2 μm and provide empirical experimental input for computational models of initiation and detonation.

The development of a mechanistic understanding of the increase in fracture risk in human bone with age is essential to public health. This represents a challenge for fracture mechanics as bone has a complex, hierarchical structure with characteristic features ranging from nanometer to macroscopic dimensions, and is thus much more complex than most engineering materials. In this study, we review ex vivo fracture experiments which quantitatively assess the effect of age on human cortical bone in the proximal-distal orientation, i.e. along the long axis of the bone. Specifically, cortical bone is seen to exhibit rising crack-growth resistance with crack extension; the toughness is consequently evaluated in terms of R-curves, measured in bones taken from a wide range of age groups (34-99 years). Both crack-initiation and crack-growth toughnesses were determined and were found to deteriorate with age; the initiation toughness decreases some 40% over the 65 years of ageing, while 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. This explanation is supported by an examination of the micro-/nanostructural changes accompanying the process of ageing, performed using deep-UV Raman spectroscopy, computed X-ray tomography and optical/ electron microscopy.

The present paper reports results of monotonic tensile and of fatigue testing of an aligned monofilament composite SiC–Al. Macroscopic measures of damage (changes in unloading compliance and in unrecovered strain) correlate with noninvasive X-ray microCT (microtomography) quantification of microstructure (alteration of fibre separation, fibre misorientation relative to the load axis and amount of fibre fracture). Monotonic loading beyond yield (188 MPa) alters fibre arrangement and reduces fibre misorientation. Fracture of fibre carbon cores begins at 828 MPa and increases rapidly with rising stress concomitant with marked unloading modulus decreases and permanent strain increases. Fatigue at 621 MPa produces gradually increasing modulus and unrecovered strain with no evidence of fibre damage. At low cycles, the modulus, permanent strain and fraction of fractured C cores increase while fibre misorientation decreases; above 16 cycles, modulus decreases with gradual increases in the other quantities...

The aging-related deterioration of the fracture properties of bone, coupled with higher life expectancy, is responsible for increasing incidence of bone fracture in the elderly; consequently, an understanding of how these fracture properties degrade with age is essential. In this study, ex vivo fracture experiments have been performed to quantitatively assess the effect of age on human cortical bone in the proximal–distal orientation, i.e., longitudinally along the osteons. Because cortical bone exhibits rising crack-growth resistance with crack extension, 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 crack-initiation and crack-growth toughness are determined and are found to deteriorate with age; the initiation toughness decreases some 40% over six 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. An examination of the micro-/nano-structural changes accompanying the process of aging, using optical microscopy, X-ray tomography, nanoindentation and Raman spectroscopy, is shown to support such observations.

The morphology and microstructure induced in high quality fused silica by UV (355 nm) laser pulses at high fluence (10–45 J/cm 2 ) have been investigated using a suite of microscopic and spectroscopic tools. The laser beam has a near-Gaussian profile with a 1/e 2 diameter of� 0.98 mm at the sample plane and a pulse length FWHM (full width at half maximum) of 7.5 ns. The damage craters consist of a molten core region (thermal explosion), surrounded by a near concentric region of fractured material. The latter arises from propagation of lateral cracks induced by the laser-generated shock waves, which also compact the crater wall,� 10 lm thick and� 20% higher in density. The size of the damage crater varies with laser fluence, number of pulses, and laser irradiation history. In the compaction layer, there is no detectable change in the Si/O stoichiometry to within ±1.6% and no crystalline nano-particles of Si were observed. Micro(1–10 lm) and nano- (20–200 nm) cracks are found, however. A lower valence Si 3+ species on the top 2–3 nm of the compaction layer is evident from the Si 2p XPS. The results are used to construct a physical model of the damage crater and to gain critical insight into laser damage process. � 2005 Elsevier B.V. All rights reserved. PACS: 61.80.Ba; 61.72.Ji; 78.60.Hk; 76.30.Mi

This study compares changes in bone microstructure in 6-month-old male GC-treated and female ovariectomized mice to their respective controls. In addition to a reduction in trabecular bone volume, GC treatment reduced bone mineral and elastic modulus of bone adjacent to osteocytes that was not observed in control mice nor estrogen-deficient mice. These microstructural changes in combination with the macrostructural changes could amplify the bone fragility in this metabolic bone disease.Patients with glucocorticoid (GC)-induced secondary osteoporosis tend to fracture at higher bone mineral densities than patients with postmenopausal osteoporosis. This suggests that GCs may alter bone material properties in addition to BMD and bone macrostructure.Changes in trabecular bone structure, elastic modulus, and mineral to matrix ratio of the fifth lumbar vertebrae was assessed in prednisolone-treated mice and placebo-treated controls for comparison with estrogen-deficient mice and sham-operated controls. Compression testing of the third lumbar vertebrae was performed to assess whole bone strength.Significant reductions in trabecular bone volume and whole bone strength occurred in both prednisolone-treated and estrogen-deficient mice compared with controls after 21 days (p0.05). The average elastic modulus over the entire surface of each trabecula was similar in all the experimental groups. However, localized changes within the trabeculae in areas surrounding the osteocyte lacunae were observed only in the prednisolone-treated mice. The size of the osteocyte lacunae was increased, reduced elastic modulus around the lacunae was observed, and a "halo" of hypomineralized bone surrounding the lacunae was observed. This was associated with reduced (nearly 40%) mineral to matrix ratio determined by Raman microspectroscopy. These localized changes in elastic modulus and bone mineral to matrix ratio were not observed in the other three experimental groups.Based on these results, it seems that GCs may have direct effects on osteocytes, resulting in a modification of their microenvironment. These changes, including an enlargement of their lacunar space and the generation of a surrounding sphere of hypomineralized bone, seem to produce highly localized changes in bone material properties that may influence fracture risk.

The calculation of the scalar compressive and shear anisotropy factors developed for single crystal refractory compounds has been adapted to the anisotropic elastic stiffness coefficients determined by a number of ultrasonic measurements of bone based on transverse isotropic symmetry. Later, this work was extended to include the ultrasonic measurements of bone based on orthotropic symmetry. Recently, the five transverse isotropic elastic constants for both wet and dry human dentin were determined using resonant ultrasound spectroscopy. The five transverse isotropic elastic constants for wet bovine enamel and dentin had been calculated based on modeling of ultrasonic wave propagation measurements and related data in the literature. The scalar compressive and shear anisotropy factors have been calculated from both these sets of data and are compared with a representative set from those published previously for both human and bovine bone and both fluoro- and hydroxyl-apatites.

Many fractures occur in teeth that have been altered, for example restored or endodontically repaired. It is therefore essential to evaluate the structure and mechanical properties of these altered dentins. One such altered form of dentin is transparent (sometimes called sclerotic) dentin, which forms gradually with aging. The present study focuses on differences in the structure and mechanical properties of normal versus transparent dentin. The mineral concentration, as measured by X-ray computed microtomography, was significantly higher in transparent dentin, the elevated concentration being consistent with the closure of the tubule lumens. Crystallite size, as measured by small angle X-ray scattering, was slightly smaller in transparent dentin, although the importance of this finding requires further study. The elastic properties were unchanged by transparency; however, transparent dentin, unlike normal dentin, exhibited almost no yielding before failure. In addition, the fracture toughness was lowered by roughly 20% while the fatigue lifetime was deleteriously affected at high stress levels. These results are discussed in terms of the altered microstructure of transparent dentin.

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.

The fracture of bone is a health concern of increasing significance as the population ages. It is therefore of importance to understand the mechanics and mechanisms of how bone fails, both from a perspective of outright (catastrophic) fracture and from delayed/time-dependent (subcritical) cracking. To address this need, there have been many in vitro studies to date that have attempted to evaluate the relevant fracture and fatigue properties of human cortical bone; despite these efforts, however, a complete understanding of the mechanistic aspects of bone failure, which spans macroscopic to nanoscale dimensions, is still lacking. This paper seeks to provide an overview of the current state of knowledge of the fracture and fatigue of cortical bone, and to address these issues, whenever possible, in the context of the hierarchical structure of bone. One objective is thus to provide a mechanistic interpretation of how cortical bone fails. A second objective is to develop a framework by which fracture and fatigue results in bone can be presented. While most studies on bone fracture have relied on linear-elastic fracture mechanics to determine a single-value fracture toughness (e.g., K c or G c ), more recently, it has become apparent that, as with many composites or toughened ceramics, the toughness of bone is best described in terms of a resistance-curve (R-curve), where the toughness is evaluated with increasing crack extension. Through the use of the R-curve, the intrinsic and extrinsic factors affecting its toughness are separately addressed, where 'intrinsic' refers to the damage processes that are associated with crack growth ahead of the tip, and 'extrinsic' refers to the shielding mechanisms that primarily act in the crack wake. Furthermore, fatigue failure in bone is presented from both a classical fatigue life (S/N) and fatigue-crack propagation (da/dN) perspective, the latter providing for an easier interpretation of fatigue micromechanisms. Finally, factors, such as age, species, orientation, and location, are discussed in terms of their effect on fracture and fatigue behaviour and the associated mechanisms of bone failure.

We describe a new method for quantifying the orientation of trabecular bone from three-dimensional images. Trabecular lattices from five human vertebrae were decomposed into individual trabecular elements, and the orientation, mass, and thickness of each element were recorded. Continuous functions that described the total mass (M(phi,theta)) and mean thickness (tau(phi,theta)) of all trabeculae as a function of orientation were derived. The results were compared with experimental measurements of the elastic modulus in three principal anatomic directions. A power law scaling relationship between the anisotropies in mass and elastic modulus was observed; the scaling exponent was 1.41 (R2=0.88). As expected, the preponderance of trabecular mass was oriented along the cranial-caudal direction; on average, there was 3.4 times more mass oriented vertically than horizontally. Moreover, the vertical trabeculae were 30% thicker, on average, than the horizontal trabeculae. The vertical trabecular thickness was inversely related to connectivity (R2=0.70; P=0.07), suggesting a possible organization into either few, thick trabeculae or many thin trabeculae. The method, which accounts for the mechanical connectedness of the lattice, provides a rapid way to both visualize and quantify the three-dimensional organization of trabecular bone.

The mechanical properties of SCS-6 SiC fibers were measured as a function of fiber radius using nanoindentation techniques. Hardness and Young's modulus were characterized for the material in all of the major regions of these fibers: the carbon core, the graphitic core coating, the inner SiC sheath, and the outer SiC sheath. The carbon core of the fibers was determined to be uniform in properties but extremely compliant. Young's modulus of 28 GPa and a hardness of 4.2 GPa were measured. The graphitic core coating was found to exhibit considerable anelasticity and to have both a low modulus (21 GPa) and a low hardness (1.7 GPa). The inner sheath of the fiber, which contained a varying chemistry, showed a sharp increase in stiffness and hardness from the inner core. Modulus and hardness increased by an order of magnitude over just 1 or 2 μm when transversing radially away from the core into the SiC. This change in properties was pronounced and clearly defined. The outer sheath, which contained a uniform chemistry and microstructure, was consistently stiff and hard when transversing radially. The average modulus and hardness for the full fiber was 333 GPa. The values reported for Young's modulus and hardness clearly showed that the mechanical properties of SCS SiC fibers exhibit dramatic changes across their diameters.

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.

Human dentin is susceptible to failure under repetitive cyclic-fatigue loading. This investigation seeks to address the paucity of data that reliably quantify this phenomenon. Specifically, the effect of alternating vs. mean stresses, characterized by the stress- or load-ratio R (ratio of minimum-to-maximum stress), was investigated for three R values (−1, 0.1, and 0.5). Dentin was observed to be prone to fatigue failure under cyclic stresses, with susceptibility varying, depending upon the stress level. The “stress-life” ( S/N) data obtained are discussed in the context of constant-life diagrams for fatigue failure. The results provide the first fatigue data for human dentin under tension-compression loading and serve to map out safe and unsafe regimes for failure over a wide range of in vitro fatigue lives (< 103to > 106cycles).

It is widely held that the hardness and modulus of dentin increase in proportion to the mineral concentration. To test this belief, we measured hardness and modulus of normal dentin and an altered form of dentin without gap-zone mineralization in wet and dry conditions by AFM nanoindentation to determine if the modulus and hardness scale linearly with mineral concentration. Mineral concentrations in the mid-coronal location of the normal and altered dentins were 44.4 vol% and 30.9 vol%, respectively. Surrounding the pulp of the altered dentin was a region of higher mineralization, 40.5 vol%. The indentation modulus of normal dentin was 23.9 (SD = 1.1) GPa dry and 20.0 (SD = 1.0) GPa wet. In mid-coronal regions of the altered dentin, the indentation modulus was 13.8 (SD = 2.0) GPa dry and 5.7 (SD = 1.4) GPa wet. In the more mineralized regions of the altered dentin, the modulus was 20.4 (SD = 1.8) GPa dry and 5.3 (SD = 0.8) GPa wet; the properties of the altered wet dentin did not correlate with mineral concentration. The results of this study raise doubt as to whether mineral concentration alone is a sufficient endpoint for assessing the success or failure of remineralization approaches in restorative dentistry.

Osteoporosis is a syndrome of excessive skeletal fragility that results from both the loss of trabecular bone mass and trabecular bone connectivity. Recently, bFGF has been found to increase trabecular bone mass in osteoporotic rats. The purpose of this study was to compare how trabecular bone architecture, bone cell activity, and strength are altered by two different bone anabolic agents, bFGF and hPTH(1–34), in an osteopenic rat model. Materials and Methods: Six-month-old female Sprague-Dawley rats (n = 74) were ovariectomized (OVX) or sham-operated (sham) and maintained untreated for 2 months. Then OVX rats were subcutaneously injected with basic fibroblast factor (bFGF; 1 mg/kg, 5 days/week), human parathyroid hormone [hPTH(1–34); 40 μg/kg, 5 days/week], or vehicle for 60 days (days 60–120 ). Sham-operated and one group of OVX animals were injected with vehicle. Biochemical markers of bone turnover (urinary deoxypyridinoline cross-links; Quidel Corp., San Diego, CA, USA) and serum osteocalcin (Biomedical Technologies, Stroughton, MA, USA) were obtained at study days 0, 60, 90, and 120 and analyzed by ELISA. At death, the right proximal tibial metaphysis was removed, and microcomputed tomography was performed for trabecular bone structure and processed for histomorphometry to assess bone cell activity. The left proximal tibia was used for nanoindentation/mechanical testing of individual trabeculae. The data were analyzed with Kruskal Wallis and post hoc testing as needed. Results: Ovariectomy at day 60 resulted in about a 50% loss of trabecular bone volume compared with sham-treated animals. By day 120 post-OVX, OVX + vehicle treated animals had decreased trabecular bone volume, connectivity, number, and high bone turnover compared with sham-operated animals [p < 0.05 from sham-, hPTH(1–34)-, and bFGF-treated groups]. Treatment of OVX animals with bFGF and hPTH(1–34) both increased trabecular bone mass, but hPTH(1–34) increased trabecular thickness and bFGF increased trabecular number and connectivity. Histomorphometry revealed increased mineralizing surface and bone formation rate in both bFGF and hPTH(1–34) animals. However, osteoid volume was greater in bFGF-treated animals compared with both the hPTH(1–34) and OVX + vehicle animals (p < 0.05). Nanoindentation by atomic force microscope was performed on approximately 20 individual trabeculae per animal (three animals per group) and demonstrated that elastic modulus and hardness of the trabeculae in bFGF-treated animals were similar to that of the hPTH-treated and sham + vehicle-treated animals. Conclusion: Both hPTH(1–34) and bFGF are anabolic agents in the osteopenic female rat. However, hPTH(1–34) increases trabecular bone volume primarily by thickening existing trabeculae, whereas bFGF adds trabecular bone mass through increasing trabecular number and trabecular connectivity. These results suggest the possibility of sequential treatment paradigms for severe osteoporosis.

Despite substantial clinical interest in the frac- ture resistance of human dentin, there is little mechanistic information in archival literature that can be usefully used to model such fracture. In fact, although the fracture event in dentin, akin to other mineralized tissues like bone, is widely believed to be locally strain-controlled, there has never been any scientific proof to support this belief. The present study seeks to address this issue through the use of a novel set of in vitro experiments in Hanks' balanced salt solution involv- ing a double-notched bend test geometry, which is designed to discern whether the critical failure events involved in the onset of fracture are locally stress- or strain-controlled. Such experiments are further used to characterize the notion of "plasticity" in dentin and the interaction of cracks with the salient microstructural features. It is observed that fracture in dentin is indeed locally strain-controlled and that the presence of dentinal tubules does not substantially affect this process of crack initiation and growth. The results pre- sented are believed to be critical steps in the development of a micromechanical model for the fracture of human dentin that takes into consideration the influence of both the mi- crostructure and the local failure mode. © 2003 Wiley Peri- odicals, Inc. J Biomed Mater Res 67A: 484 - 495, 2003

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.

The finite element method, which has been successfully applied to studies of the elastic properties of trabecular bone, is now being used to simulate its failure. These simulations have used a geometrically linear (linear kinematic) approximation to the total stiffness matrix; nonlinear terms in the total stiffness matrix have been excluded from the computation in order to achieve efficiency. Because trabecular bone appears to be a slender (i.e., geometrically nonlinear) structure, we studied the validity of the linear kinematic approximation for simulating its failure. Two cases, designed to bracket the extremes of stability behavior, were explored: a single representative spicule of trabecular bone (case 1) and a volume of trabecular bone consisting of relatively low aspect ratio members (case 2). For case 1, geometrically linear (GL) and nonlinear (GNL) analyses were performed with two different materials models: a plastic damage model and a brittle damage model. When GNL terms were included in the total stiffness matrix, we found that load-path bifurcation preceded tissue failure regardless of the form of the damage model. This bifurcation was the result of a complex coupling between material yield and structural instability. The nature of this coupling was highly sensitive to the form of the damage model. None of these behaviors was observed in the linear analyses, where failure was insensitive to the form of the damage model and where structural instabilities were prevented from occurring. For case 2, compressive loading of a volume of trabecular bone, geometric nonlinear effects were pronounced. There was a bifurcation in load response that resulted in large apparent strain to failure. The GL simulations, on the other hand, precluded this bifurcation. We hypothesize that trabecular bone is a geometric nonlinear structure; nonlinear terms must be included in the total stiffness matrix to accurately simulate its failure.

Osteoporosis is a disease of excess bone fragility that results from both the loss of bone mass and trabecular bone microarchitecture, thereby creating a very fragile skeleton. The purpose of this study was to determine whether treatment of ovariectomized (OVX) osteopenic rats with basic fibroblast growth factor (bFGF) would stimulate the production of new trabeculae, and whether the newly formed trabeculae would make physical connections with the pre-existing trabeculae after prolonged estrogen deficiency. Six-month-old Sprague Dawley rats were OVXed or sham-operated and were left untreated until day 60 post-OVX. A high resolution microscopic scan (XTM) of the right proximal tibia was performed on groups 1 and 2 on day 1 post-OVX, and was repeated in all animals on day 60 post-OVX. At day 60 groups 1 and 2 were treated with vehicle and groups 3 to 6 were injected with bFGF 200 microg/kg/d intravenously for 15 days. At day 82, all animals obtained another in vivo XTM scan of the right tibia; then group 4 were treated with 17B estradiol 10 microg/kg/3x a week, group 5 were treated with hPTH (1-34) at 80 microg/kg/d for 35 days, group 6 were sacrificed, and groups 1 and 2 were treated with vehicle injections for 35 days. At day 110, all remaining animals were sacrificed, and repeat ex vivo XTM scans of the right proximal tibia were performed. Trabecular bone structural variables-including trabecular bone volume, connectivity, number, and thickness-were obtained from all XTM scans. Biochemical markers of bone turnover were also obtained 24 hours before each XTM scan (osteocalcin and deoxypyridinoline), and analyzed by ELISA. Animals OVXed and treated with vehicle had decreased trabecular bone volume, connectivity and number compared to sham-operated animals at both day 60 and day 110. Animals treated with bFGF from day 60-75 post-OVX had evidence of new trabeculae that physically connected with pre-existing trabeculae and also of increased trabecular bone volume seven days after the injections were discontinued. Biochemical markers of bone formation had a small and insignificant increase over baseline levels during the bFGF injections. Bone resorption markers were significantly reduced during the injection period, but returned to baseline levels after the injections were stopped. In addition, we also demonstrated that these newly formed trabecular connections could be maintained or added to with either estrogen or hPTH (1-34) treatments. Thirty-five days after ending the bFGF treatment, trabecular bone volume and connectivity was 25-80% higher in the estrogen and hPTH (1-34) treated animals compared to the untreated animals ( p0.01). These results support continued development of bFGF as a potential treatment for severely osteoporotic individuals.

The past 50 years of research on the mechanical properties of human dentin are reviewed. Since the body of work in this field is highly inconsistent, it was often necessary to re-analyze prior studies, when possible, and to re-assess them within the framework of composite mechanics and dentin structure. A critical re-evaluation of the literature indicates that the magnitudes of the elastic constants of dentin must be revised considerably upward. The Young's and shear moduli lie between 20-25 GPa and 7-10 GPa, respectively. Viscoelastic behavior (time-dependent stress relaxation) measurably reduces these values at strain rates of physiological relevance; the reduced modulus (infinite relaxation time) is about 12 GPa. Furthermore, it appears as if the elastic properties are anisotropic (not the same in all directions); sonic methods detect hexagonal anisotropy, although its magnitude appears to be small. Strength data are re-interpreted within the framework of the Weibull distribution function. The large coefficients of variation cited in all strength studies can then be understood in terms of a distribution of flaws within the dentin specimens. The apparent size-effect in the tensile and shear strength data has its origins in this flaw distribution, and can be quantified by the Weibull analysis. Finally, the relatively few fracture mechanics and fatigue studies are discussed. Dentin has a fatigue limit. For stresses smaller than the normal stresses of mastication, approximately 30 MPa, a flaw-free dentin specimen apparently will not fail. However, a more conservative approach based on fatigue crack growth rates indicates that if there is a pre-existing flaw of sufficient size (approximately 0.3-1.0 mm), it can grow to catastrophic proportion with cyclic loading at stresses below 30 MPa.

Dentin structure and properties are known to vary with orientation and location. The present study explored the variation in the ultimate tensile strength (UTS) of dentin with location in the tooth. Hourglass specimens were prepared from dentin located in the center, under cusps, and in the cervical regions of human molar teeth. These were tested in tension at various distances from the pulp. Median tensile strengths ranged from 44.4 MPa in the inner dentin near the pulp, to 97.8 MPa near the dentino-enamel junction (DEJ). This increase in the median UTS with distance from the pulp to the DEJ was statistically significant (P

NaOCl aq is used as a cleansing and non-specific deproteinizing agent in endodontic treatment, as a component of new chemomechanical caries treatment, and is under study for its alterations of dentin bonding characteristics. We sought to determine the microstructural and nanomechanical changes with such treatments and to test if NaOCl aq removed dentin collagen without microstructural or nanomechanical alteration of underlying mineralized dentin. Polished human dentin disks were prepared with a double reference technique that allowed changes to be determined following 10% citric acid etching for 15 s and subsequent treatment of the etched and unetched portions of the sample with 6.5% NaOCl aq , using atomic force microscopy (AFM) (Nanoscope III, Digital Instruments, Santa Barbara, CA). Images and measurements were made at intervals up to 1800 s. A Triboscope (Hysitron, Minneapolis, MN) on the AFM was used to measure nanohardness and the reduced elastic modulus. The double reference method allowed measurements immediately following etching and at intervals during deproteinization. Etching caused deep peritubular dentin removal and a small depth change of hydrated intertubular dentin as mineral was removed and left a remnant collagen matrix. NaOCl aq removed collagen over time, during which individual fibrils could be resolved; the underlying mineralized dentin was left with a unique porous surface containing numerous channels that are not normally observed in etched or fractured dentin. This could provide an attractive bonding substrate because of the increased surface area and high mineral content, if toughness is not reduced too much. Nanomechanical measurements showed that the reduced elastic modulus and hardness were 75% of original values after removal of the exposed collagen. Current dentin bonding systems rely on hybrid layer formation in which hydrophilic primers/polymers penetrate the opened collagen matrix exposed by etching. However some research suggests that preventing hybrid layer formation by deproteinization, in some cases, can give good bonding, and as shown here, alters the substrate microstructure. There are significant changes as indicated by ANOVA in the reduced elastic modulus that require further study to determine if these changes might affect clinical efficacy.

Item does not contain fulltext High-resolution synchrotron radiation computed tomography (SRCT) and small-angle x-ray scattering (SAXS) were performed on normal and dentinogenesis imperfecta type II (DI-II) teeth. The SRCT showed that the mineral concentration was 33% lower on average in the DI-II dentin with respect to normal dentin. The SAXS spectra from normal dentin exhibited low-angle diffraction peaks at harmonics of 67.6 nm, consistent with nucleation and growth of the apatite phase within gaps in the collagen fibrils (intrafibrillar mineralization). In contrast, the low-angle peaks were almost non-existent in the DI-II dentin. Crystallite thickness was independent of location in both DI-II and normal dentin, although the crystallites were significantly thicker in DI-II dentin (6.8 nm [SD = 0.5] vs. 5.1 nm [SD = 0.6]). The shape factor of the crystallites, as determined by SAXS, showed a continuous progression in normal dentin from roughly one-dimensional (needle-like) near the pulp to two-dimensional (plate-like) near the dentin-enamel junction. The crystallites in DI-II dentin, on the other hand, remained needle-like throughout. The above observations are consistent with an absence of intrafibrillar mineral in DI-II dentin.

The mechanical and optical properties of healthy and transparent root dentin are compared using atomic force microscopy (AFM), micro-Raman and emission spectroscopies and fluorescence microscopy. The elastic modulus and hardness of intertubular and peritubular transparent and healthy dentin did not differ appreciably. The tubule filling material in the transparent zone, however, exhibited values between peritubular and intertubular dentin. Raman spectroscopy revealed a shift in the 1066 cm−1 band to 1072 cm−1 from normal to transparent intertubular dentin. The material filling the tubule lumen in transparent dentin showed an increase in frequency of the band near 1070 cm−1 as well. The emission spectral characteristics under 351 nm photoexcitation indicate differences between normal and transparent intertubular dentin. A transition region of about 300 μm between normal and transparent dentin was identified. In this region the intertubular emission properties were the same as for normal dentin, but tubules were filled. The filling material had emission characteristics closer to the normal intertubular than to transparent intertubular dentin. © 2001 Kluwer Academic Publishers

We applied two-dimensional numerical methods to describe the spatial arrangement of tubules in human dentin. The methods considered were two-point correlation functions, entropy-like measures, and angular distributions between nearest neighbors. The correlation functions were based on Fourier transform methods. The latter two approaches were based on stochastic geometry, and involved developing the Delaunay tessellations of the tubule patterns and their dual Voronoi diagrams. We discovered that for analyzing the distribution of tubules the geometric methods of lattice tessellations were more sensitive to structural order of the tubules than were Fourier-based schemes. Analysis of the data indicated that dentinal tubules are highly ordered in normal dentin. © 2001 Kluwer Academic Publishers

Specimens of silica-reinforced polysiloxane foam pads were three-dimensionally imaged during axial compressive loading to densification. The foams' behavior was highly nonlinear and showed the three characteristic regions of linear elastic, elastic buckling, and densification. A finite-element technique, based upon conversion of the image voxels to finite elements, was used to calculate the mechanical properties of the foams. The results were compared with conventional mechanical testing and theory. The finite-element calculations were in excellent agreement with experimental stress–strain data over the entire range of compressive loading. Theoretical models, on the other hand, overestimated the stiffness of the foam above the elastic buckling stress by not correctly predicting the abruptness of the transition from elastic buckling to densification. Three-dimensional analysis of the deformed microstructures indicated that there was a critical foam density beyond which the cell morphology suddenly changed from open-celled to closed-celled and that this “phase”-like transition was responsible for the abrupt increase in stiffness near densification. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 80: 1746–1755, 2001

This article summarizes the results of a three-dimensional study of changes in the morphology of the L6 rat vertebra at 120 days after ovariectomy (OVX), with estrogen replacement therapy used as a positive control. Synchrotron radiation microtomography was used to quantify the structural parameters defining trabecular bone architecture, while finite-element methods were used to explore the relationships between these parameters and the compressive elastic behavior of the vertebrae. There was a 22% decrease in trabecular bone volume (TBV) and a 19% decline in mean trabecular thickness (Tb.Th) with OVX. This was accompanied by a 150% increase in trabecular connectivity, a result of the perforation of trabecular plates. Finite-element analysis of the trabecular bone removed from the cortical shell showed a 37% decline in the Young's modulus in compression after OVX with no appreciable change in the estrogen-treated group. The intact vertebrae (containing its trabecular bone) exhibited a 15% decrease in modulus with OVX, but this decline lacked statistical significance. OVX-induced changes in the trabecular architecture were different from those that have been observed in the proximal tibia. This difference was a consequence of the much more platelike structure of the trabecular bone in the vertebra.

Earlier, crack opening as a function of position within an optically–opaque notched tensile sample (NT–3) of Al–Li 2090 was reported for four loads by Guvenilir and co–workers; these measurements were made with high resolution X–ray computed tomography. This paper reports the same type of results for a second notched tensile sample (NT–4): the authors believe this to be the second sample whose crack closure was quantified as a function of position. The crack within NT–4 was found to be more planar than and to close differently than that in NT–3. In NT–4, the crack ‘zippe’ shut from the tip; this is in contrast to the earlier results on the asperity– dominated crack in NT–3 where contact occured primarily behind the open crack tip. During unloading of NT–4, the crack faces came into contact above the closure load defined by the intersection of tangent lines to the upper and lower portions of the load–deflection curve; this is similar to previous observations in sample NT–3. Estimates of d a /d N as a function of Δ K for samples NT–3 and NT–4 agree with other’ measurements, which suggests that the closure observations of this paper also apply to compact tension samples of Al–Li 2090.

Ultrasound has been proposed as a means to noninvasively assess bone and, particularly, bone strength and fracture risk. Although there has been some success in this application, there is still much that is unknown regarding the propagation of ultrasound through bone. Because strength and fracture risk are a function of both bone mineral density and architectural structure, this study was carried out to examine how architecture and density interact in ultrasound propagation. Due to the difficulties inherent in obtaining fresh bone specimens and associated architectural and density features, simulation methods were used to explore the interactions of ultrasound with bone. A sample of calcaneal trabecular bone was scanned with micro-CT and subjected to morphological image processing (erosions and dilations) operations to obtain a total of 15 three-dimensional (3-D) data sets. Fifteen two-dimensional (2-D) slices obtained from the 3-D data sets were then analyzed to evaluate their respective architectures and densities. The architecture was characterized through the fabric feature, and the density was represented in terms of the bone volume fraction. Computer simulations of ultrasonic propagation through each of the 15 2-D bone slices were carried out, and the ultrasonic velocity and mean frequency of the received waveforms were evaluated. Results demonstrate that ultrasound propagation is affected by both density and architecture, although there was not a simple linear correlation between the relative degree of structural anisotropy with the ultrasound measurements. This study elucidates further aspects of propagation of ultrasound through bone, and demonstrates as well as the power of computational methods for ultrasound research in general and tissue and bone characterization in particular.

This paper describes the application of synchrotron radiation microtomography to osteoporosis research. By taking advantage of the high intensity, collimation, and monochromaticity of synchrotron radiation, we have been able to image the three-dimensional trabecular bone structure in living rats, thus providing serial data on the earliest architectural changes that occur with estrogen loss. Results from these in vivo animal experiments demonstrate that one of the earliest manifestations of estrogen loss, in addition to a decrease in the amount of trabecular bone, is decreased connectivity. We demonstrate that estrogen replacement therapy, when initiated soon after significant changes have occurred, restores bone mass to baseline levels but does not recover the trabecular connectivity. Even without an associated recovery in trabecular connectivity, finite element calculations on the three-dimensional images suggest that estrogen recovers the original structural modulus of elasticity. We believe the recovery of the elastic properties is due to an increase in trabecular thickness above baseline values.

An image texture measure based on the box counting algorithm is evaluated for its potential to characterize human trabecular bone structure in medical images. Although bone images lack the self-similarity of theoretical fractals, bone images are candidates for characterization using fractal analysis because of their highly complex structure. The fractal based measure, herein called the box counting dimension (BCD), is an effective dimension, and does not imply an underlying fractal geometry. The importance of resolution in quantifying bone characteristics using the BCD is addressed. The relationship of BCD to standard measures of trabecular bone structure is also analyzed. To evaluate the variability of the BCD with change in resolution, the BCD is determined for two sections from each of seven 3D X-ray Tomographic Microscopy (XTM) images of human radius bone specimens, while the resolution is varied using lowpass filtering. An automated method of choosing the range of scales for the fractal analysis curve regression is used. The relationship of BCD to trabecular bone width and spacing is analyzed both for the XTM images and for simulated images representing idealized structures. The range of BCD values is 1.21–1.54. Variation in BCD over a range of resolutions is found to be small compared to the variation in BCD between different bone specimens. Maximum change in BCD over a large range of resolutions (17.60–176 microns per pixel) is 0.08. BCD decreases as space between trabeculae increases. Fractal based texture measures may potentially allow clinical monitoring of changes in bone structure — for example, using Magnetic Resonance Imaging at 150–200 micron resolution.

Using an atomic force microscope (AFM) with an attachment specifically designed for indentation, we measured the mechanical properties of demineralized human dentin under three conditions: in water, in air after desiccation, and in water after rehydration. The static elastic modulus (E(h)r = 134 kPa) and viscoelastic responses (tau(epsilon) = 5.1 s and tau(sigma) = 6.6 s) of the hydrated, demineralized collagen scaffolding were determined from the standard linear solid model of viscoelasticity. No significant variation of these properties was observed with location. On desiccation, the samples showed considerably larger elastic moduli (2 GPa), and a hardness value of 0.2 GPa was measured. Upon rehydration the elastic modulus decreased but did not fully recover to the value prior to dehydration (381 kPa).

Composite preform fiber architectures range from the very simple to the complex, and the extremes are typified by parallel continuous fibers and complicated three-dimensional woven structures. Subsequent processing of these preforms to produce dense composites may depend critically on the geometry of the interfiber porosity. The goal of this study is to fully characterize the structure of a 0°/90° cloth layup preform using x-ray tomographic microscopy (XTM). This characterization includes the measurement of intercloth channel widths and their variability, the transverse distribution of through-cloth holes, and the distribution of preform porosity. The structure of the intercloth porosity depends critically on the magnitude and direction of the offset between adjacent cloth layers. The structures observed include two-dimensional networks of open pipes linking adjacent holes, arrays of parallel one-dimensional pipes linking holes, and relatively closed channels exhibiting little structure, and these different structures would appear to offer very different resistances to gas flow through the preform. These measurements, and future measurements for different fiber architectures, will yield improved understanding of the role of preform structure on processing.

AA6101 aluminum foams (composition in weight %: Al-0.6 Mg-0.5 Si) were fabricated by using a directional solidification technique. The 3-D morphology of the foams was examined using synchrotron x-ray tomography and the results revealed relatively uniform, open-celled structures. The mechanical (compression) behavior of the foams was also characterized. The stress-strain curves exhibited a typical three-stage behavior: elastic, nearly-perfect plastic (i.e. with a stress plateau), and densification. The elastic moduli of a 10%-dense foam in the directions that are transverse and parallel to the solidification direction were measured to be 630 and 670 MPa, respectively. Theoretical calculations of the modulus using a FEM method with the element-by-element (EBE) formalism were also carried out. The calculated values of approximately 570 and 635 MPa compared favorably with the experimental data.

Dentin, the inner hard tissue of teeth, is a complex hydrated composite and forms the substrate for much of restorative dentistry. Current efforts to improve restorative and preventive dentistry involve the development of effective bonds to this tissue. Modern bonding techniques involve etching the dentin to remove the mineral portion, leaving a collagen network that can be infiltrated with a monomer and polymerized in place to form a mechanical bond. The objective of this study was to investigate the nature of the interfacial zone, called the resin-dentin interdiffusion zone, using scanning electron microscopy for characterization and thickness measurements, X-ray tomographic microscopy for fracture characteristics and atomic force microscopy for the local modulus and hardness variations.

Objectives: Dentin is a vital, hydrated composite material with structural components and properties that vary with location. These variations are reviewed along with alterations by physiological and pathological changes that allow classification into various forms of dentin. Structural characteristics and mechanical properties are reviewed and the limitations of our understanding of structure-property relationships for normal and modified forms of dentin are discussed with respect to their impact on dentin bonding. Recent progress in methods available to study dentin and its demineralization are emphasized with their promise to increase our understanding of dentin properties and structure. Data sources: Recent microstructural studies, focusing on scanning electron microscopy, atomic force microscopy and X-ray tomographic microscopy are included. A review of fundamental studies with emphasis on microstructurally sensitive methods, and prior reviews of basic mechanical properties are included with discussion of their correlation to composition and structure. Study selection and conclusions: Emphasis in this work was placed on the major structural components of the tissue, including the collagen based organic matrix and its mineral reinforcement, the distribution of these components and their microstructural organization as related to mechanical properties and response to demineralization. Little information is included on biochemical and developmental studies or on non-collagenous proteins and other organic components for which limited understanding is available with respect to their role in structure-property relations and influence on bonding. In spite of the fact that the complexity of dentin precluded a comprehensive review, it is clear that local structural variations influence properties and impact nearly all preventive and restorative dental treatments. Much more work is needed in order to understand differences between vital and non-vital dentin, and dentin from extracted teeth. Although our knowledge is rudimentary in certain areas, increasingly sophisticated methods of studying dentin should provide the necessary information to model structure-property relations, optimize dentin bonding, and improve many aspects of preventive and restorative dentistry.

Objectives This investigation sought to determine: 1) if dentin demineralization rates are proportional to acid concentration for demineralization in phosphoric acid (10% or 1.76M, 0.025M, 0.0001 M, with pH=0.95, 2.0, 4.0 respectively); 2) if the etching characteristics are independent of dentin depth; and 3) if the etching characteristics for phosphoric acid were comparable to those for citric acid over a similar pH range. Methods Highly polished dentin disks from freshly extracted, non-carious, third molars were prepared with a reference layer. Samples were prepared from either superficial or deep coronal dentin. The samples were etched for periods of up to 30 min using phosphoric acid solutions (pH = 0.95, 2.0, 4.0) in a wet cell of an atomic force microscope (AFM). Depth changes with respect to the reference layer were determined for the intertubular and peritubular dentin to quantify structural changes. The results were compared with similar studies using citric acid (pH = 1.0, 2.15 or 3.4). Etching characteristics were statistically compared using 2-way repeated measures ANOVA at p Results The relation between time and recession for peritubular dentin was initially linear. The intertubular dentin recession started rapidly but then reached a plateau within a very short interval for etching solutions at pH = 2.0 and 4.0. At the highest concentration, the recession decreased with time, but a clear plateau was not established. There was no statistical difference between peritubular etching rates of superficial and deep dentin surfaces with phosphoric acid at any concentration. There was also no difference in the intertubular dentin recession at the location of the plateau that depended on dentin depth. Etching rates increased dramatically with decreased pH for both phosphoric and citric acids, but were higher for citric acid than for phosphoric acid. Significance The AFM allowed quantification of changes during etching of wet dentin. Peritubular dentin etching rates increased with decreasing pH, as expected, but changes were not linear and were different for the two acids studied over a similar pH range. Intertubular dentin surface recession was small and plateaued for low concentrations. The peritubular etching rate and intertubular dentin recession did not depend on dentin depth.

Lattice models for calculating the elastic properties of cellular structures are described; on small scales the elastic constants are isotropic, both in two and three dimensions. Stresses are transmitted by harmonic springs that connect the nodes surrounding each volume element. The force constants of the springs are determined by the local elastic stiffness, which can vary from element to element. The model was tested by comparing the elastic constants of periodic two-dimensional microstructures with analytic results. Then it was applied to calculations of the elastic constants of samples of human trabecular bone, using images of the microstructure determined by X-ray transmission microscopy.

Results of in situ high resolution X-ray computed tomography are reported for a notched tensile sample of AlLi 2090 T841. The fatigue crack within the interior of the sample is imaged with 6 μm voxels as a function of applied load, and the crack face morphology is found to be similar to that observed in compact tension samples of this alloy. The loads and approximate stress intensities at which the tomography data were obtained were 82, 50, 25 and 5 kg and 7.1, 4.3, 2.2 and 0.4 MPa√m, respectively. Crack openings measured during unloading as a function of position show that physical closure at portions of the crack tip and at positions behind the crack tip precedes (during unloading) the bend in the sample's load-displacement curve. The three-dimensional pattern of crack opening shows substantial mixed mode I–III contact on the faces of asperities behind the crack tip, even at the maximum load of the fatigue cycle. Mixed mode I–II contact is also observed at loads above the bend in the load-displacement curve. The fraction of voxels open remains nearly constant for the loads immediately above and below the nominal closure load, as determined from the load-displacement curve, of 41 kg; and this suggests that these mixed mode I–III surfaces begin to carry significant load at the point where the load-displacement curve starts to deflect, and is the source of the apparent stiffening of the sample at loads below the nominal closure load.

Human dentin is known to be susceptible to failure under cyclic loading. Surprisingly, there are few reports that quantify the effect of such loading, considering the fact that a typical tooth experiences a million or so loading cycles annually. In the present study, a systematic investigation is described of the effects of prolonged cyclic loading on human dentin in a simulated physiological environment. In vitro stress-life (S/N) data are discussed in the context of possible mechanisms of fatigue damage and failure.

The contribution of trabecular bone structure to bone strength is of considerable interest in the study of osteoporosis and other disorders characterized by changes in the skeletal system. Magnetic resonance (MR) imaging of trabecular bone has emerged as a promising technique for assessing trabecular bone structure. In this in vitro study we compare the measures of trabecular structure obtained using MR imaging and higher-resolution X-ray tomographic microscopy (XTM) imaging of cubes from human distal radii. The XTM image resolution is similar to that obtained from histomorphometric sections (18 microns isotropic), while the MR images are obtained at a resolution comparable to that achievable in vivo (156 x 156 x 300 microns). Standard histomorphometric measures, such as trabecular bone area fraction (synonymous with BV/TV), trabecular width, trabecular spacing and trabecular number, texture-related measures and three-dimensional connectivity (first Betti number/volume) of the trabecular network have been derived from these images. The variation in these parameters as a function of resolution, and the relationship between the structural parameters, bone mineral density and the elastic modulus are also examined. In MR images, because the resolution is comparable to the trabecular dimensions, partial volume effects occur, which complicate the segmentation of the image into bone and marrow phases. Using a standardized thresholding criterion for all images we find that there is an overestimation of trabecular bone area fraction (approximately 3 times), trabecular width (approximately 3 times), fractal dimension (approximately 1.4 times) and first Betti number/ volume (approximately 10 times), and an underestimation of trabecular spacing (approximately 1.6 times) in the MR images compared with the 18-microns XTM images. However, even for a factor of 9 difference in spatial resolution, the differences in the morphological trabecular structure measures ranged from a factor of 1.4 to 3.0. We have found that trabecular width, area fraction, number, fractal dimension and Betti number/volume measured from the XTM and MR images increases, while trabecular spacing decreases, as the bone mineral density and elastic modulus increase. A preliminary bivariate analysis showed that in addition to bone mineral density alone, the Betti number, trabecular number and spacing contributed to the prediction of the elastic modulus. This preliminary study indicates that measures of trabecular bone structure using MR imaging may play a role in the study of osteoporosis.

A specially modified atomic-force microscope was used to measure the hardness of fully hydrated peritubular and intertubular dentine at two locations within unerupted human third molars: within 1 mm of the dentine enamel junction and within 1 mm of the pulp. The hardness of fully hydrated peritubular dentine was independent of location, and ranged from 2.23 to 2.54 GPa. The hardness of fully hydrated intertubular dentine did depend upon location, and was significantly greater near the dentine enamel junction (values ranged from 0.49 to 0.52 GPa) than near the pulp (0.12-0.18 GPa). A Nanoindenter was used to estimate the Young's modulus of dehydrated peritubular and intertubular dentine from the unloading portion of the load displacement curve. The modulus values averaged 29.8 GPa for the peritubular dentine (considered to be a lower limit), and ranged from 17.7 to 21.1 GPa for the intertubular dentine, with the lower values obtained for dentine near the pulp.

Metal/ceramic interfaces play a critical role in determining the mechanical behavior of composite materials. In metal-matrix composites (MMCs), the presence of the reinforcing phase places the normally ductile matrix phase in a highly constrained state of stress. Strong interfaces between matrix and reinforcement favor crack advance by ductile rupture of the metal, while weak interfaces favor debonding. In practice, the introduction of reinforcements into a metal produces a variability in behavior that limits its commercial application. Because of this, micromechanics models of failure have been developed for these systems that attempt to describe the failure mechanisms. The authors have experimentally duplicated the simplified geometry of the micromechanics models and subjected the specimens to a well defined stress state in bending. The bend tests were interrupted and XTM was performed to reveal the mechanism of crack extension.

Dentin conditioners provide a microporous surface for penetration by bonding agents. This study used an atomic force microscope (AFM) to examine the initial steps in the conditioning process of dentin using three demineralizing agents, 0.5 M EDTA, and dilute solutions of phosphoric (3mM, 6mM) and citric (5 mM) acids, in order to establish the relationships between demineralization and changes in surface morphology. Polished dentin disks had a 10-nm-thick gold pattern applied which served as a height reference. Samples(n = 3/agent) were examined at baseline and at 2-s intervals for up to 120 s for each agent. EDTA (0.5 M) was used as received; other conditioners were diluted to slow the rates of demineralization for detailed study. The surfaces of the peritubular and intertubular regions were altered differently. Initially subsidence rates were equal and linear, but after a 100-nm depth change the intertubular rates decreased. For phosphoric acid and citric acid, the movement of the intertubular surface was uniform and the surfaces remained smooth. However, the intertubular surfaces were rough for the EDTA treatment. The surface subsidence reached a plateau after a depth change of about 0.5μm, which resulted from a limit to the contraction of the demineralized and hydrated collagen scaffold. © 1995 John Wiley & Sons, Inc.

Many bonding agents require the dentin surface to be acid-etched prior to being bonded. Understanding the stability and morphology of the etched dentin surface is important for improving bond strength and reliability in these systems. In this study, the atomic force microscope was used to quantify dimensional changes that occur to fully hydrated dentin during demineralization with a pH 4.0 lactic acid gel. A high-resolution microtomography instrument, the x-ray tomographic microscope, was also used to quantify the mineral density distribution in the dentin as a function of etching time. The intertubular dentin surface shrank by less than 0.5 μm during etching, while the peritubular dentin receded at an initially rapid linear rate. The dentin surface retained its initial morphology, although it was more porous with the removal of the peritubular dentin. Beneath the etched surface, there were three major zones characterized by mineral density differences. The first zone was a fully demineralized collagen layer, subjacent to which was a partially demineralized zone of roughly constant mineral density. Immediately following the partially mineralized layer was normal dentin. The presence of the partially mineralized layer could be explained in terms of different transport rates in the peritubular and intertubular dentin.