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Instruments / Technical Area	Publication Details	Published
I22-Small angle scattering & Diffraction	Association between nanoscale strains and tissue level nanoindentation properties in age-related hip-fractures Andrea Bonicelli , Tabitha Tay , Justin P. Cobb , Oliver R. Boughton , Ulrich Hansen , Richard L. Abel , Peter Zioupos Journal Of The Mechanical Behavior Of Biomedical Materials 81 DOI: 10.1016/j.jmbbm.2022.105573 Diamond Proposal Number(s): [17664, 13337] Open Access Show Abstract ▼ Abstract: Measurement of the properties of bone as a material can happen in various length scales in its hierarchical and composite structure. The aim of this study was to test the tissue level properties of clinically-relevant human bone samples which were collected from donors belonging to three groups: ageing donors who suffered no fractures (Control); untreated fracture patients (Fx-Untreated) and patient who experienced hip fracture despite being treated with bisphosphonates (Fx-BisTreated). Tissue level properties were assessed by (a) nanoindentation and (b) synchrotron tensile tests (STT) where strains were measured at the ‘tissue’, ‘fibril’ and ‘mineral’ levels by using simultaneous Wide-angle - (WAXD) and Small angle- X-ray diffraction (SAXD). The composition was analysed by thermogravimetric analysis and material level endo- and exo-thermic reactions by differential scanning calorimetry (TGA/DSC3+). Irrespective of treatment fracture donors exhibited significantly lower tissue, fibril and mineral strain at the micro and nanoscale respectively and had a higher mineral content than controls. In nanoindentation only nanohardness was significantly greater for Controls and Fx-BisTreated versus Fx-Untreated. The other nanoindentation parameters did not vary significantly across the three groups. There was a highly significant positive correlation (p < 0.001) between organic content and tissue level strain behaviour. Overall hip-fractures were associated with lower STT nanostrains and it was behaviour measured by STT which proved to be a more effective approach for predicting fracture risk because evidently it was able to demonstrate the mechanical deficit for the bone tissue of the donors who had experienced fractures.	Nov 2022
I22-Small angle scattering & Diffraction	Nanoscale mechanisms in age-related hip-fractures Shaocheng Ma , En Lin Goh , Tabitha Tay , Crispin C. Wiles , Oliver Boughton , John H. Churchwell , Yong Wu , Angelo Karunaratne , Rajarshi Bhattacharya , Nick Terrill , Justin P. Cobb , Ulrich Hansen , Richard L. Abel Scientific Reports 10 DOI: 10.1038/s41598-020-69783-5 Diamond Proposal Number(s): [17664] Open Access Show Abstract ▼ Abstract: Nanoscale mineralized collagen fibrils may be important determinants of whole-bone mechanical properties and contribute to the risk of age-related fractures. In a cross-sectional study nano- and tissue-level mechanics were compared across trabecular sections from the proximal femora of three groups (n = 10 each): ageing non-fractured donors (Controls); untreated fracture patients (Fx-Untreated); bisphosphonate-treated fracture patients (Fx-BisTreated). Collagen fibril, mineral and tissue mechanics were measured using synchrotron X-Ray diffraction of bone sections under load. Mechanical data were compared across groups, and tissue-level data were regressed against nano. Compared to controls fracture patients exhibited significantly lower critical tissue strain, max strain and normalized strength, with lower peak fibril and mineral strain. Bisphosphonate-treated exhibited the lowest properties. In all three groups, peak mineral strain coincided with maximum tissue strength (i.e. ultimate stress), whilst peak fibril strain occurred afterwards (i.e. higher tissue strain). Tissue strain and strength were positively and strongly correlated with peak fibril and mineral strains. Age-related fractures were associated with lower peak fibril and mineral strain irrespective of treatment. Indicating earlier mineral disengagement and the subsequent onset of fibril sliding is one of the key mechanisms leading to fracture. Treatments for fragility should target collagen-mineral interactions to restore nano-scale strain to that of healthy bone.	Aug 2020
I22-Small angle scattering & Diffraction	The changes in bone's nanostructure associated with bone fragility & bisphosphonate treatment Tabitha Jia Hui Tay Open Access Show Abstract ▼ Abstract: The contribution of the nanostructure to whole bone strength has long been debated. However the impact of the collagen-mineral matrix on whole bone mechanics has yet to be tested. At the start of the study, bone volume and microarchitecture were found to not entirely account for bone strength, even though new ITS techniques were included, and thus it seemed possible that the gap could be attributed to the nanostructure. State-of-the-art synchrotron imaging was used to compare nanomechanics between bones from ageing non-fracture donors and ageing fracture patients, half of whom had been prescribed bisphosphonate. Fracture patients exhibited with lower tissue, collagen and mineral strains than non-fracture patients, suggesting that their nanostructures were less deformable. In addition, the fracture patients exhibited with wider mineral crystals, providing for larger surface areas for interfacial bonding with collagen fibrils, and thus preventing the unwinding and sliding of the matrix during loading. The less deformable matrix may reduce macroscopic strength via a cascade effect by easier initiation and growth of microcracks in the collagen-mineral matrix and limiting the bone’s ability to bend and absorb energy during a trip or fall. This new knowledge of the importance of the nanoscale deformation to whole bone strength could fill gaps in current diagnostics and treatments, if it were possible to measure deformation properties in vivo. Nanoindentation was developed to measure such deformations, and as such, a benchtop system was used to measure material properties of the three groups, and the data was correlated with nanostrain data. However, nanoindentation material properties and fibril and mineral strains were not correlated. In addition to the lack of correlation to microstructure and macro level strength and stiffness, it seems that nanoindentation does not measure material properties accurately and thus other alternatives need to be looked into for in-vivo measurements at the nanoscale.	Jun 2020

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