Ultrastructure of Bone: Hierarchical Features from Nanometer to Micrometer Scale Revealed in Focused Ion Beam Sections in the TEM.

The ultrastructure of bone has been widely debated, in part due to limitations in visualizing nanostructural features over relevant micrometer length scales. Here, we employ the high resolving power and compositional contrast of high-angle annular dark-field scanning transmission electron microscopy (HAADF STEM) to investigate new features in human bone with nanometer resolution over microscale areas. Using focused ion beam (FIB)-milled sections that span an area of 50 µm2, we have shown how most of the mineral of cortical human osteonal bone occurs in the form of long, thin polycrystalline plates (mineral lamellae, MLs) which are either flat or curved to wrap closely around collagen fibrils. Close to the collagen fibril (< 20 nm), the radius of curvature matches that of the fibril diameter, while at greater distances, MLs form arcs with much larger radii of curvature. In addition, stacks of closely packed planar (uncurved) MLs occur between fibrils. The curving of mineral lamellae both around and between the fibrils would contribute to the strength of bone. At a larger scale, rosette-like clusters of fibrils are noted for the first time, arranged in quasi-circular arrays that define tube-like structures in alternating osteonal lamellae. At the boundary between adjacent osteonal lamellae, the orientation of fibrils and surrounding mineral lamellae changes abruptly, resembling the "orthogonal" patterns identified by others (Reznikov et al. in Acta Biomater 10:3815-3826, 2014). These features spanning nanometer to micrometer scale have implications for our understanding of bone structure and mechanical integrity.

Influence of Substrate Heating and Nitrogen Flow on the Composition, Morphological and Mechanical Properties of SiNx Coatings Aimed for Joint Replacements.

Silicon nitride (SiNx) coatings are promising for joint replacement applications due to their high wear resistance and biocompatibility. For such coatings, a higher nitrogen content, obtained through an increased nitrogen gas supply, has been found to be beneficial in terms of a decreased dissolution rate of the coatings. The substrate temperature has also been found to affect the composition as well as the microstructure of similar coatings. The aim of this study was to investigate the effect of the substrate temperature and nitrogen flow on the coating composition, microstructure and mechanical properties. SiNx coatings were deposited onto CoCrMo discs using reactive high power impulse magnetron sputtering. During deposition, the substrate temperatures were set to 200 °C, 350 °C or 430 °C, with nitrogen-to-argon flow ratios of 0.06, 0.17 or 0.30. Scanning and transmission electron spectroscopy revealed that the coatings were homogenous and amorphous. The coatings displayed a nitrogen content of 23-48 at.% (X-ray photoelectron spectroscopy). The surface roughness was similar to uncoated CoCrMo (p = 0.25) (vertical scanning interferometry). The hardness and Young's modulus, as determined from nanoindentation, scaled with the nitrogen content of the coatings, with the hardness ranging from 12 ± 1 GPa to 26 ± 2 GPa and the Young's moduli ranging from 173 ± 8 GPa to 293 ± 18 GPa, when the nitrogen content increased from 23% to 48%. The low surface roughness and high nano-hardness are promising for applications exposed to wear, such as joint implants.

Surface and Subsurface Analyses of Metal-on-Polyethylene Total Hip Replacement Retrievals.

Metal-on-polyethylene (MoP) articulations are one of the most reliable implanted hip prostheses. Unfortunately, long-term failure remains an obstacle to the service life. There is a lack of higher resolution research investigating the metallic surface component of MoP hip implants. This study investigates the surface and subsurface features of metallic cobalt chromium molybdenum alloy (CoCrMo) femoral head components from failed MoP retrievals. Unused prostheses were used for comparison to differentiate between wear-induced defects and imperfections incurred during implant manufacturing. The predominant scratch morphology observed on the non-implanted references was shallow and linear, whereas the scratches on the retrievals consisted of largely nonlinear, irregular scratches of varying depth (up to 150 nm in retrievals and up to 60 nm in reference samples). Characteristic hard phases were observed on the surface and subsurface material of the cast samples. Across all samples, a 100-400 nm thick nanocrystalline layer was visible in the immediate subsurface microstructure. Although observation of the nanocrystalline layer has been reported in metal-on-metal articulations, its presence in MoP retrievals and unimplanted prostheses has not been extensively examined. The results suggest that manufacturing-induced surface and subsurface microstructural features are present in MoP hip prostheses prior to implantation and naturally, these imperfections may influence the in vivo wear processes after implantation.