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Sol-gel preparation of calcium titanium phosphate: viscosity, thermal properties and solubility
(2012)
Calcium titanium phosphate (CTP) was prepared by the sol–gel route in order to prepare suitable coatings. This work addresses the question of how to prepare stable CTP sols. Their rheological properties as a function of process parameters like solid loading and water content are investigated. It was found that an increased solid loading as well as an increased water content lead to an increased initial viscosity as well as a more pronounced ageing induced viscosity rise. In addition, the thermal behavior of the resulting xerogels was analyzed. Furthermore, we studied the ion release behavior of the xerogels when brought in contact with water. Results suggest that calcium titanium phosphate shows a diffusion controlled ion release mode with a preferential release of Ca.
Solubility and ingrowth behaviour of degradable and figuline calcium alkaline phosphate cements
(2012)
The thrust of the investigations presented here is to point out the degradation behaviour in vitro and the ingrowth behaviour in vivo of four different calcium alkaline phosphate cements. Two of the figuline and mouldable composites consist of the crystalline phase Ca2KNa(PO4)2 and two of the crystalline phase Ca10[K/Na](PO4)2 each containing 2wt% medium gel strength porcine gelatin. Furthermore A-TCP was added to both Ca10[K/Na](PO4)2 cements as a hardening supporting reactant. The testing material groups differ in small amorphous portions containing either silica phosphate (GB9), magnesium potassium phosphate (GB14) or diphosphates (401545 and 401545(70)). The respective composites show a monomodal particle size distribution (d50~7µm; span~4) and an average total porosity around 28vol%.For the solubility studies cylindrical samples (d=6mm; h=12mm) were stored in a 0.1mol TRIS buffer solution and incubated at 37°C for maximum 50 weeks. The storage solution was analysed and renewed every week. The results are plotted cumulative. For the in vivo studies critical size defects were dissected to mandibles in a sheep model in which a 1cm³ area of the bottom of the mandibles was surgically resected and replaced with the figuline cements whereas the mouldability allows the reconstruction of the original outer contour without draining off even when replacing upside down.
Selective laser sintering of ceramic powders is a promising technique for the additive manufacturing of complex- and delicate-shaped ceramic parts. Most techniques have in common that the powder to be sintered is spread to a thin layer as a dry powder by means of a roller or shaker system. These layers have a relatively low density. On the other hand, appreciable densities can be reached with the use of ceramic slurries as the starting material. Therefore, the layer-wise slurry deposition (LSD) process has been developed. Layer stacks, i.e. powder beds, built up by employing the LSD technology exhibit a density comparable to ceramic powder compacts processed by means of conventional forming technologies. Writing the layer information with a focused laser beam in these dense ceramic powder compacts enables the manufacture of ceramic bodies with a high density and precision in contour.
This study suggests a tool for a better control on the sintering/crystallization of 3D-printed bioactive glassceramics bodies. A small cantilever in form of a bar with square cross section attached to a base and inclined 34◦ with the horizon, was used to monitor the viscous flow and sintering/crystallization headway of a glassceramic systems. 3D printing and sintering of bioactive glass-ceramics is of great interest for medical care applications.
Viscous flow ensures sufficient densification of the typically low density printed green bodies, while crystallization prevents the structure from collapsing under the gravitational load. As a model system, a bioactive glass called BP1 (48.4 SiO2, 1 B2O3, 2 P2O5, 36.6 CaO, 6.6 K2O, 5.6 Na2O (mol%)), which has a chemical composition based on that of ICIE16, was employed in this work. In addition, ICIE16 was used as a reference glass. The results show that the suggested design is a very promising tool to track the real-time deformation of 3D printed glass-ceramic specimens and gives a good indication for the onset of crystallization as well.