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Synchrotron radiation-based microcomputed tomography (SR-µCT) has become a valuable tool in the
structural characterization of different types of materials, achieving volumetric details with micrometre
resolution. Biomedical research dealing with porous polymeric biomaterials is one of the research fields
which can benefit greatly from the use of SR-µCT. This study demonstrates that current experimental setups
at synchrotron beamlines achieve a sufficiently high resolution in order to visualize the positions of
individual cartilage cells cultivated on porous gelatine scaffolds made by a freeze-structuring technique.
Depending on the processing parameters, the pore morphology of the scaffolds investigated was changed
from large-pore sized but non-ordered structures to highly directional and fine pored. The cell-seeded
scaffolds were stained with a combined Au/Ag stain to enhance the absorption contrast in SR-µCT. While
only some cells showed enhanced absorption contrast, most cells did not show any difference in contrast
to the surrounding scaffold and were consequently not detectable using conventional greyscale threshold
methods. Therefore, using an image-based three-dimensional segmentation tool on the tomographic data
revealed a multitude of non-stained cells. In addition, the SR-µCT data were compared with data obtained
from scanning electron microscopy, energy dispersive X-ray spectroscopy and histology, while further
linking the initial cell density measured via a MTT assay to the pore size as determined by SR-µCT.
Current light microscopic methods such as serial sectioning, confocal microscopy or multiphoton microscopy are severely limited in their ability to analyse rather opaque biological structures in three dimensions, while electron optical methods offer either a good three-dimensional topographic visualization (scanning electron microscopy) or high-resolution imaging of very thin samples (transmission electron microscopy). However, sample preparation commonly results in a significant alteration and the destruction of the three-dimensional integrity of the specimen. Depending on the selected photon energy, the interaction between X-rays and biological matter provides semi-transparency of the specimen, allowing penetration of even large specimens. Based on the projection-slice theorem, angular projections can be used for tomographic imaging. This method is well developed in medical and materials science for structure sizes down to several micrometres and is considered as being non-destructive. Achieving a spatial and structural resolution that is sufficient for the imaging of cells inside biological tissues is difficult due to several experimental conditions. A major problem that cannot be resolved with conventional X-ray sources are the low differences in density and absorption contrast of cells and the surrounding tissue. Therefore, X-ray monochromatization coupled with a sufficiently high photon flux and coherent beam properties are key requirements and currently only possible with synchrotron-produced X-rays. In this study, we report on the three-dimensional morphological characterization of articular cartilage using synchrotron-generated X-rays demonstrating the spatial distribution of single cells inside the tissue and their quantification, while comparing our findings to conventional histological techniques.
Tribological screening tests (simple, reciprocating ball-on-flat tests) were performed with the objective to identify an appropriate coating for the articulating surfaces of artificial hip joints whose acetabular cups and femoral stems are made from Ti6Al4V alloy, which is appreciated for its light weight, good biocompatibility and elastic properties similar to those of natural bone. Standard coatings like TiN or CrN performed better than more complicated multi-layer systems, though not as good as different types of amorphous carbon coatings, generally referred to as diamond-like carbon or DLC coatings. Among the latter, hydrogenated amorphous carbon (a-C:H) displayed the best properties, especially if the hydrogen content was increased by reducing the bias voltage during PA-CVD-deposition.
The optimised a-C:H coating revealed the most promising wear behaviour under the applied testing conditions, i.e. the increase of linear wear with the number of cycles was close to zero. Regarding the materials examined in this study, correlation of wear with mechanical properties obtained by nano-indentation revealed that high hardness was not an adequate criterion for selecting appropriate coatings. A high ratio of hardness and elastic modulus (H/E) proved to be more important. Microstructural and micro-analytical investigations revealed transformation of TiN and CrN to TiO2 and Cr2O3, respectively, and amorphous carbon was, at least partly, transformed to graphite. Furthermore, incorporation of Al2O3 from the ball was observed at a very fine scale. The wear debris of favourable coatings always formed agglomerates of nano-scale particles. It was shown that commercial nano-particles of Al2O3, Cr2O3 and carbon black are comparable to particles generated by the tribological tests. However, it is uncertain whether they are comparable to those formed during simulator studies or in vivo. Furthermore, the performance of the favourable coating has to be tested in a hip joint simulator before its potential for application in prostheses can be assessed.
Cr3+-doped MgF2 systems are synthesised by a novel non-aqueous soft chemistry route using different Cr precursors and varying Cr loading. These systems have been characterized by X-ray powder diffraction (XRD), BET surface area, TPD of ammonia, FT-IR pyridine adsorption analysis and X-ray photoelectron spectroscopy, and tested for their catalytic activity in dismutation of CCl2F2 and CF3CHClF. Catalysts synthesised starting from CrO3 or (CH3CO2)7Cr3(OH)2 showed better catalytic activity than those prepared with CrCl3. FT-IR pyridine adsorption studies reveal that the catalytic activity is highly correlated with the Lewis acid strength. In TPD of NH3 catalysts prepared from CrO3 and (CH3CO2)7Cr3(OH)2, precursors showed a similar behaviour, different from that of catalysts prepared from CrCl3.
Cr3+-doped MgF2 systems are synthesised by a novel non-aqueous soft chemistry route using different Cr precursors and varying Cr loading. These systems have been characterized by X-ray powder diffraction (XRD), BET surface area, TPD of ammonia, FT-IR pyridine adsorption analysis and X-ray photoelectron spectroscopy, and tested for their catalytic activity in dismutation of CCl2F2 and CF3CHClF. Catalysts synthesised starting from CrO3 or (CH3CO2)7Cr3(OH)2 showed better catalytic activity than those prepared with CrCl3. FT-IR pyridine adsorption studies reveal that the catalytic activity is highly correlated with the Lewis acid strength. In TPD of NH3 catalysts prepared from CrO3 and (CH3CO2)7Cr3(OH)2, precursors showed a similar behaviour, different from that of catalysts prepared from CrCl3.