Boom Clay is considered as one of the potential host rocks for the disposal of high level and/or long lived radioactive waste in a geological formation in Belgium (Mol study site, Mol-1 borehole) and the Netherlands. The direct characterisation of the pore space is essential to help understand the transport properties of radionuclides in argillaceous materials.This contribution aims to characterise and compare the morphology of the pore space in different Boom Clay samples, representing end-members with regard to mineralogy (i.e. clay content) and grain-size distribution of this formation. Broad ion beam (BIB) cross-sectioning is combined with SEM imaging of porosity and Mercury injection Porosimetry (MIP) to characterise the variability of the pore space in Boom Clay at the nm- to μm-scale within representative 2D areas and to relate microstructural observations to fluid flow properties of the bulk sample material. Segmented pores in 2D BIB surfaces are classified according to the mineralogy, generating representative datasets of up to 100,000 pores per cross-section.Results show total SEM-resolved porosities of 10-20% and different characteristic mineral phase internal pore morphologies and intra-phase porosities.Most of the nano-porosity resides in the clay matrix. In addition, in the silt-rich samples, larger inter-aggregate pores contribute to a major part of the resolved porosity. Pore-size distributions within the clay matrix suggest power-law behaviour of pore areas with exponents between 1.56-1.74. Mercury injection Porosimetry, with access to pore-throat diameters down to 3.6 nm, shows total interconnected porosities between 27-35 Vol.-%, and the observed hysteresis in the MIP intrusion vs. extrusion curves suggests relatively high pore-body to pore-throat ratios in Boom Clay. The difference between BIB-SEM visible and MIP measured porosities is explained by the resolution limit of the BIB-SEM method, as well as the limited size of the BIB-polished cross-section areas analysed. Compilation of the results provides a conceptual model of the pore network in fine- and coarse-grained samples of Boom Clay, where different mineral phases show characteristic internal porosities and pore morphologies and the overall pore space can be modelled based on the distribution of these mineral phases, as well as the grain-size distribution of the samples investigated.

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Study of the pore space in mudstones by mercury intrusion porosimetry is a common but indirect technique and it is not clear which part of the pore space is actually filled with mercury. We studied samples from the Opalinus Clay, Boom Clay, Haynesville Shale, and Bossier Shale Formations using Wood's metal injection at 316 MPa, followed by novel ion beam polishing and high-resolution scanning electron microscopy. This method allowed us to analyze at high resolution which parts of a rock are intruded by the liquid alloy at mm to cm scale. Results from the Opalinus Clay and Haynesville Shale show Wood's Metal in cracks, but the majority of the pore space is not filled although mercury intrusion data suggests that this is the case. In the silt-rich Boom Clay sample, the majority of the pore space was filled Wood's metal, with unfilled islands of smaller pores. Bossier Shale shows heterogeneous impregnation with local filling of pores as small as 10 nm. We infer that mercury intrusion data from these samples is partly due to crack filling and compression of the sample. This compaction is caused by effective stress developed by mercury pressure and capillary resistance; it can close small pore throats, prevent injection of the liquid metal, and indicate an apparent porosity. Our results suggest that many published MIP data on mudstones could contain serious artifacts and reliable metal intrusion porosimetry requires a demonstration that the metal has entered the pores, for example by Wood's metal injection, broad ion beam polishing, and scanning electron microscopy.

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