J.D. Almer

Synchrotron X-ray diffraction study of load partitioning during elastic deformation of bovine dentin.

The elastic properties of dentin, a biological composite consisting of stiff hydroxyapatite (HAP) nano-platelets within a compliant collagen matrix, are determined by the volume fraction of these two phases and the load transfer between them. We have measured the elastic strains in situ within the HAP phase of bovine dentine by high energy X-ray diffraction for a series of static compressive stresses at ambient temperature. The apparent HAP elastic modulus (ratio of applied stress to elastic HAP strain) was found to be 18+/-2GPa. This value is significantly lower than the value of 44GPa predicted by the lower bound load transfer Voigt model, using HAP and collagen volume fractions determined by thermo-gravimetric analysis. This discrepancy is explained by (i) a reduction in the intrinsic Youngs modulus of the nano-size HAP platelets due to the high fraction of interfacial volume and (ii) an increase in local stresses due to stress concentration around the dentin tubules.

Effect of high-energy X-ray doses on bone elastic properties and residual strains.

Bone X-ray irradiation occurs during medical treatments, sterilization of allografts, space travel and in vitro studies. High doses are known to affect the post-yield properties of bone, but their effect on the bone elastic properties is unclear. The effect of such doses on the mineral-organic interface has also not been adequately addressed. Here, the evolution of elastic properties and residual strains with increasing synchrotron X-ray dose (5-3880 kGy) is examined on bovine cortical bone. It is found that these doses affect neither the degree of nanometer-level load transfer between the hydroxyapatite (HAP) platelets and the collagen up to stresses of -60 MPa nor the microscopic modulus of collagen fibrils (both measured by synchrotron X-ray scattering during repeated in situ loading and unloading). However, the residual elastic strains in the HAP phase decrease markedly with increased irradiation, indicating damage at the HAP-collagen interface. The HAP residual strain also decreases after repeated loading/unloading cycles. These observations can be explained by temporary de-bonding at the HAP/collagen interface (thus reducing the residual strain), followed by rapid re-bonding (so that load transfer capability is not affected).

Evolution of load transfer between hydroxyapatite and collagen during creep deformation of bone

While the matrix/reinforcement load-transfer occurring at the micro- and nanoscale in nonbiological composites subjected to creep deformation is well understood, this topic has been little studied in biological composites such as bone. Here, for the first time in bone, the mechanisms of time-dependent load transfer occurring at the nanoscale between the collagen phase and the hydroxyapatite (HAP) platelets are studied. Bovine cortical bone samples are subjected to synchrotron X-ray diffraction to measure in situ the evolution of elastic strains in the crystalline HAP phase and the evolution of viscoelastic strains accumulating in the mineralized collagen fibrils under creep conditions at body temperature. For a constant compressive stress, both types of strains increase linearly with time. This suggests that bone, as it deforms macroscopically, is behaving as a traditional composite, shedding load from the more compliant, viscoelastic collagen matrix to the reinforcing elastic HAP platelets. This behavior is modeled by finite-element simulation carried out at the fibrillar level.

Variability in the elastic properties of bovine dentin at multiple length scales

Various methods are used to investigate the variability in elastic properties across a population of deciduous bovine incisor root dentin samples spanning different animals, incisor types, and locations within teeth. First, measurements of elastic strains by high-energy synchrotron X-ray scattering during compressive loading of dentin specimens provided the effective modulus--the ratio of applied stress to elastic phase strain--for the two main phases of dentin (hydroxyapatite crystals and mineralized collagen fibrils), shedding light on load transfer operating at the nanoscale between collagen and mineral phases. Second, Youngs moduli were measured at the macroscale by ultrasonic time-of-flight measurements. Third, thermogravimetry quantified the volume fractions of hydroxyapatite, protein and water at the macroscale. Finally, micro-Computed Tomography determined spatial variations of the mineral at the sub-millimeter scale. Statistical comparison of the above properties reveals: (i) no significant differences for dentin samples taken from different animals or different incisor types but (ii) significant differences for samples taken from the cervical or apical root sections as well as from different locations between buccal and lingual edges.

Variability in the nanoscale deformation of hydroxyapatite during compressive loading in bovine bone.

High-energy synchrotron X-ray diffraction is used to study in situ elastic strains in hydroxyapatite (HAP) for bovine femur cortical bone subjected to uniaxial compressive loading. Load-unload tests at room temperature (27°C) and body temperature (37°C) show that the load transfer to the stiff nanosized HAP platelets from the surrounding compliant protein matrix does not vary significantly (p<0.05) with temperature. This emphasizes that the stiffness of bone is controlled by the stiffness of the HAP phase, which remains unaffected by this change in temperature. Both the extent of hysteresis and the residual value of internal strains developed in HAP during load-unload cycling from 0 to -100 MPa increase significantly (p<0.05) with the number of loading cycles, indicative of strain energy dissipation and accumulation of permanent deformation. Monotonic loading tests, conducted at body temperature to determine the spatial variation of properties within the femur, illustrate that the HAP phase carries lower strain (and thus stresses) at the anterio-medial aspect of the femur than at the anterio-lateral aspect. This is correlated to higher HAP volume fractions in the former location (p<0.05). The Youngs modulus of the bone is also found to correlate with the HAP volume fraction and porosity (p<0.05). Finally, samples with a primarily plexiform microstructure are found to be stiffer than those with a primarily Haversian microstructure (p<0.05).

Lattice strains and load partitioning in bovine trabecular bone.

Microdamage and failure mechanisms have been well characterized in bovine trabecular bone. However, little is known about how elastic strains develop in the apatite crystals of the trabecular struts and their relationship with different deformation mechanisms. In this study, wide-angle high-energy synchrotron X-ray diffraction has been used to determine bulk elastic strains under in situ compression. Dehydrated bone is compared to hydrated bone in terms of their response to load. During compression, load is initially borne by trabeculae aligned parallel to loading direction with non-parallel trabeculae deforming by bending. Ineffective load partitioning is noted in dehydrated bone whereas hydrated bone behaves like a plastically yielding foam.

In-situ stress analysis of multilayer environmental barrier coatings.

The biaxial stress and thermal expansion of multilayer doped-aluminosilicate environmental barrier coatings were measured in situ during cooling using microfocused high-energy X-rays in transmission. Coating stresses during cooling from 1000 °C were measured for as-sprayed and thermally cycled samples. In the as-sprayed state, tensile stresses as high as 75 MPa were measured in the doped-aluminosilicate topcoat at 375 °C, after which a drop in the stress occurred accompanied by through-thickness cracking of the two outermost layers. After thermally cycling the samples, the stress in the topcoat was reduced to approximately 50 MPa, and there was no drop in stress upon cooling. This stress reduction was attributed to a crystallographic phase transformation of the topcoat and the accompanying change in thermal expansion coefficient. The addition of a doped aluminosilicate to the mullite layer did not lower the stress in the topcoat, but may offer increased durability due to an increased compressive stress.

Separating the recrystallization and deformation texture components by high-energy X-rays

High-energy synchrotron diffraction offers great potential for experimental study of recrystallization kinetics. Measurements on partially recrystallized samples using a monochromatic high-energy synchrotron beam show that recrystallized grains generate sharp diffraction spots, whereas the intensity from the deformed matrix varies smoothly along the Debye–Scherrer rings. Based on these observations, a method has been developed to separate the recrystallization texture components from those originating from the deformation matrix. The validity of this method is demonstrated with partially recrystallized interstitial-free steel.

Nondestructive Strain Tensor Scanning within Samples of Cylindrical Symmetry

The radial (i.e., depth below the surface) dependence of the residual strain tensor within shot‐peened samples of cylindrical geometry is measured nondestructively using high‐energy synchrotron radiation (80 keV). Transmission geometry is employed in combination with a triangulation slit and area detector. Thus, a radial gauge length is defined directly by the beam size rather than cumulatively as in conventional reflection geometry. A narrow incident beam of 30 micrometer diameter is used, and we demonstrate that macroscopic grain averaging is achieved even in the bulk, where the grain size is large, by oscillating the samples in two dimensions. Therefore, the samples are rotated with high frequency around the cylinder axis and translated with low frequency parallel to the axis. We argue that the combination of a narrow incident beam, a two‐dimensional sample oscillation, and area detector provides a versatile technique to overcome insufficient grain averaging as the gauge volumes can be flexibly chosen ...

Synchrotron radiation study on alloy 617 and alloy 230 for VHTR application

High-energy synchrotron radiation has proven to be a powerful technique for investigating fundamental deformation processes for various materials, particularly metals and alloys. In this study, high-energy synchrotron X-ray diffraction (XRD) was used to evaluate Alloy 617 and Alloy 230, both of which are top candidate structural materials for the Very-High-Temperature Reactor (VHTR). Uniaxial tensile experiments using in-situ high-energy X-ray exposure showed the substantial advantages of this synchrotron technique. First, the small volume fractions of carbides, e.g. ∼6% of M6 C in Alloy 230, which are difficult to observe using lab-based X-ray machines or neutron scattering facilities, were successfully examined using high-energy X-ray diffraction. Second, the loading processes of the austenitic matrix and carbides were separately studied by analyzing their respective lattice strain evolutions. In the present study, the focus was placed on Alloy 230. Although the Bragg reflections from the γ matrix behave differently, the lattice strain measured from these reflections responds linearly to external applied stress. In contrast, the lattice strain evolution for carbides is more complicated. During the transition from the elastic to the plastic regime, carbide particles experience a dramatic loading process, and their internal stress rapidly reaches the maximum value that can be withstood. The internal stress for the particles then decreases slowly with increasing applied stress. This indicates a continued particle fracture process during plastic deformations of the γ matrix. The study showed that high-energy synchrotron X-ray radiation, as a non-destructive technique for in-situ measurement, can be applied to ongoing material research for nuclear applications.Copyright