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Analyse morphologique de la microstructure 3D de réfractaires électrofondus à très haute teneur en zircone : relations avec les propriétés mécaniques, chimiques et le comportement pendant la transformation quadratique-monoclinique

Abstract : Zirconia-Rich Fused-Cast Refractories are largely used in industry to build glass furnaces. This kind of refractory is composed of two phases: a dendritic skeleton of zirconia surrounded by a glassy phase which represents about 12% in volume. This work aims to evaluate the influences of the 3D microstructural morphology and of the properties of the constituting phases on the mechanical properties of materials, especially during the transformation from tetragonal to monoclinic which occurs during cooling-down after casting. This work is part of the NOREV (New refractories for glass furnaces) project funded by the French ANR (National Agency for Research). 3D pictures of the microstructures have been obtained owing to X-ray microtomographies performed at ESRF (European Synchrotron Radiation Facility, Grenoble, France). After segmentation, these images allowed the microstructural topology of materials to be investigated, using image analysis and mathematical morphology parameters like covariance, tortuosity and percolation. A relationship between the surface density of the zirconia skeleton and its dissolution kinetics in hydrofluoric acid (HF) solution has been identified. Segmenting the skeleton using the watershed method allowed the connectivities of the different materials to be compared. The results are correlated with the numerical calculations of the microstructure stiffness. A phenomenon of flexibility of the zirconia skeleton has been observed on thin specimens, at high temperature and at room temperature, when the glassy phase has been removed. This phenomenon is related to the connectivity and to the “puzzle-like” structure of the zirconia skeleton. Dilatometric measurements revealed the effects of yttrine addition. The glassy phase exhibits a very important role in the t-m transformation, while limiting microstructural damage of materials. The refractory containing 7% yttrine revealed properties totally different from other materials: its stiffness is higher and it does not experience the t-m transformation. 3D finite element simulations have been carried out on elementary volumes of the actual microstructure of the materials. The influences of the properties of the constituting phases, of the microstructural morphology and of the boundary conditions, which are responsible for the microstructural damage during cooling down, could then be estimated.
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Yang Ding. Analyse morphologique de la microstructure 3D de réfractaires électrofondus à très haute teneur en zircone : relations avec les propriétés mécaniques, chimiques et le comportement pendant la transformation quadratique-monoclinique. Autre. Ecole Nationale Supérieure des Mines de Paris, 2012. Français. ⟨NNT : 2012ENMP0031⟩. ⟨pastel-00743511⟩

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