Effect of X-ray irradiation on the elastic strain evolution in the mineral phase of bovine bone under creep and load-free conditions

Both the load partitioning between hydroxyapatite (HAP) and collagen during compressive creep deformation of bone and the HAP residual strain in unloaded bone have been shown in previous synchrotron X-ray diffraction studies to be affected by the X-ray irradiation dose. Here, through detailed analysis of the X-ray diffraction patterns of bovine bone, the effect of X-ray dose on (i) the rate of HAP elastic strain accumulation/shedding under creep conditions and (ii) the HAP lattice spacing and average root mean square (RMS) strain under load-free conditions are examined. These strain measurements exhibit three stages in response to increasing X-ray dose. Up to ∼75 kGy (stage I) no effect of dose is observed, indicating a threshold behavior. Between ∼75 and ∼300 kGy (stage II) in unloaded bone the HAP d-spacing increases and the RMS strain decreases with dose, indicating strain relaxation of HAP. Furthermore, under constant compressive load creep conditions, the rate of compressive elastic strain accumulation in HAP decreases with increasing dose until, at ∼115 kGy, it changes sign, indicating that the HAP phase is shedding load during creep deformation. These stage II behaviors are consistent with HAP-collagen interfacial damage, which allows the HAP elastic strain to relax within both the loaded and unloaded samples. Finally, for doses in excess of ∼300 kGy (stage III, measured up to 7771 kGy) the HAP lattice spacing and RMS strain for load-free samples and the rate of HAP elastic strain shedding for crept samples remain independent of dose, suggesting a saturation of damage and/or stiffening of the collagen matrix due to intermolecular cross-linking.