Papers by Author: Didier Bernache-Assollant

Abstract: This work aimed at preparing dense and monophasic silicated hydroxyapatite ceramics over the range 0 ≤ x ≤ 1.0 mol of silicon. The synthesis of the powder via an aqueous precipitation process followed by an adapted thermal treatment showed that it was possible to obtain dense single-phased apatite ceramics containing up to 0.6 mol of silicon. The in vitro biological characterization of these materials was performed.

Abstract: In this study, we report on the effect of Bioglass® structural transformations on its sintering behaviour. In a previous paper, we showed that while heating up to 1000°C, five successive transformations occur: glassy transition, phase separation, two crystallization processes and a second glassy transition. The sintering of the material exhibits two main shrinkage stages associated to the two glassy transitions at 550°C and 850°C. At 580°C, the glass-in-glass phase separation induces a decrease of the sintering rate immediately followed by the crystallisation of the major phase Na2CaSi2O6 between 600 and 700°C, from the surface to the bulk of the particles. A completed inhibition of sintering takes place followed by a minor shrinkage due to volume crystallization. A plateau is observed until the second glassy transition.

Abstract: The removal of cadmium from water by fixation into a calcium phosphate apatite Ca10(PO4)6(OH)2 (CaHA) was investigated in batch experiments. These ones were carried out using a wide range of initial Cd2+ concentration, three different temperatures, and several CaHA surface areas. The amount of immobilized cadmium was proportional to the surface area of CaHA, whatever the experimental parameters might be. It could reach 7.1 mol of Cd per mol of starting CaHA. Thermal and XPS analyses on the exchanged powders proved that a part of cadmium was quickly adsorbed at the grains surface in the form of hydrated complexes [Cd(OH2)n]2+. The latter were formed by an ionic exchange between adsorbed calcium and cadmium of the solution. Adsorption reaction was mainly limited by the number of specific sites available on the grains surface. Structural analyses showed that another part of Cd was slowly incorporated into a solid solution Ca10-xCdx(PO4)6(OH)2 (CaCdHA) onto the CaHA crystals surface. Results demonstrated unambiguously that the incorporation process was a surface precipitation and not an intracrystalline diffusion.

Abstract: Sintering behaviour of monazite powder was investigated as a function of the powder milling conditions. To this aim, two techniques were used: attrition-milling and mixer-milling. We show that it is of prime importance to control all the milling parameters in order to obtain controlled microstructure and to avoid abnormal grain growth or residual large porosity.

Abstract: In this work, the hydroxyapatite was prepared from cortical bone after calcination at 700°C during 1 hour. In order to improve mechanical properties of HA, 5 wt% of the ZrO2 (stabilized with 12.0 wt% CeO2), Al2O3 and TiO2 were added to HA powder as a reinforcing phase. All the powders were sintered at 1300°C for 2 hours. The XRD was utilized to identify the phases composition. It was found that the initial calcined powder is hydroxyapatite with the following chemical composition Ca5(PO4)3OH. In addition, the phenolphthalein test has put into evidence the existence of free CaO. For powders containing ZrO2, the XRD spectra has showed a little percent of formed b-tricalcium phosphate (b-TCP); the HA was decomposed to (b-TCP) and CaO which forms with ZrO2 the calcium zirconate (CaZrO3). Nevertheless, in powders containing TiO2, the XRD spectra showed that a partial decomposition of HA to b-TCP was occurred with formation of calcium titanium oxide (CaTiO3). However, for powders containing Al2O3, a nearly full decomposition of HA to b-TCP was occurred, the free Al2O3 was present. Finally, it has been found that HA composites containing a large amount of b-tricalcium phosphate are resorbale than HA composites containing a small amount of b-TCP and they were not well densified. The microhardness values of HA- ZrO2 composites were greater than those of HA- Al2O3 and HATiO2 composites.