Abstract
Savonnières, a French layered oolithic limestone, shows important ink-bottle effects. As a consequence, a great discrepancy is observed between the results of different techniques to determine the pore volume distribution. It is shown that mercury intrusion porosimetry results can be considered as the main drainage curve and are, for this kind of materials, not convenient to determine the apparent pore volume distribution due to hysteresis phenomena. The main wetting curve is obtained using image analysing techniques on SEM-micrographs, combined with pressure membrane apparatus results on capillary saturated samples.
A simple structural hysteresis model is developed to predict the mercury intrusion porosimetry results, starting from the main wetting curve. The good agreement between theory and experiment verifies that the large difference between main wetting and main drainage curve can indeed be attributed to structural hysteresis. In this way, the presented technique gives, in addition to a better knowledge of the pore volume distribution, insight in the pore geometry and connectivity, which can serve as input for microstructure-based transport models.
Résumé
La courbe de rétention d'eau et la courbe de distribution volumique des pores obtenues au moyen de la porosimétrie à intrusion de mercure (PIM), de l'appareil à membrane de pression et des techniques d'analyse d'images sur micrographe-MEB sont comparées pour la pierre de Savonnières, une roche calcaire oolithique plus ou moins stratifiée en provenance de la France. Le matériau montre d'importants effets «bouteille d'encre». Il est démontré que les résultats obtenus par PIM peuvent être considérés comme courbe principale de drainage et ne peuvent pas être utilisés, pour ces matériaux, pour déterminer la distribution volumique apparente des pores en raison de phénomènes d'hystérésis. La courbe principale de mouillage est obtenue par des techniques d'analyse d'images sur micrographe MEB, combinées avec les résultats de l'appareil à membrane de pression sur des échantillons saturés par capillarité.
Un modèle structurel simple d'hystérésis est développé; il est capable de prédire les résultats obtenus par porosimétrie à intrusion de mercure au départ de la courbe principale de mouillage. Ceci permet de vérifier que la grande différence entre les courbes principales de mouillage et de drainage peut en effet être attribuée aux hystérésis de structure. Comme conséquence, la méthode présentée donne, outre une meilleure connaissance de la distribution volumique des pores, un aperçu de la géométrie des pores et de la connectivité, ce qui peut servir de données en entrée pour des modèles de transfert basés sur la microstructure.
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Roels, S., Elsen, J., Carmeliet, J. et al. Characterisation of pore structure by combining mercury porosimetry and micrography. Mat. Struct. 34, 76–82 (2001). https://doi.org/10.1007/BF02481555
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DOI: https://doi.org/10.1007/BF02481555