Geomechanics from Micro to Macro – Soga et al. (Eds) © 2015 Taylor & Francis Group, London, ISBN 978-1-138-02707-7 Relationships between desiccation cracking behavior and microstructure of the Tournemire clay-rock by coupling DIC and SEM methods A-L. Fauchille, S. Hedan, D. Prêt & P. Cosenza IC2MP–HydrASA, CNRS, Université de Poitiers, ENSIP Poitiers, France V. Valle Institut PPRIME CNRS, Université de Poitiers, Futuroscope Chasseneuil, France J. Cabrera DEI-SARG Department, Institute for Radiological Protection and Nuclear Safety, Fontenay-aux-Roses, France ABSTRACT: The study presented here aims to identify the microstructural factors which govern the cracking of Tournemire clay-rock caused by humidity changes. A new experimental setup was designed in laboratory to compare the location of desiccation cracks, induced by humidity changes, to the microstructure of a sample (20 × 20 × 20 mm3 ) of Tournemire clay-rock. The location of desiccation cracks was measured on a surface of 5.6 × 4.2 mm2 by Digital Image Correlation (DIC) and the microstructure was quantitatively estimated by Scanning Electron Microscopy on the same surface. First results show that at millimeter scale the desiccation cracks are divided in two parallel networks: the first network is composed of continuous macrocracks located next to local mineralogical heterogeneities such as the proportion and the mean size of grains, and the second network of discontinuous microcracks at the boundaries between grain/grain, grain/clay matrix or in clay matrix. 1 INTRODUCTION Thanks to mechanical and textural properties, the clayrocks are an interesting medium to nuclear waste disposal at great depth. An important cracking due to a desaturation process of the argillaceous medium was observed on the gallery walls of the Underground Laboratory of Tournemire (Aveyron, France). When the galleries are excavated and operated, air supplying implies humidity changes and participates to the extension of the Excavation Damaged Zone (EDZ), in which the hydric and mechanical properties of clay-rocks are modified. On the front and the walls of galleries, the cracks are organized in two networks : the principal network is sub-horizontal in the same direction that bedding planes and the second is vertical opposed to bedding planes. Their opening and their aperture are principally driven by relative humidity in the gallery (Hedan et al. 2014). At present, the mechanical and geological factors which control this fracturing are poorly understood. The study presented here aims to identify the relationship between the location of desiccation cracks and the microstructure of the rock. A sample (20 × 20 × 20 mm3 ) was submitted a cycle of shrinkage/swelling/shrinkage under controlled humidity changes (RH = 98-33-98-33%). One face was filmed by a camera to follow the evolution of the cracks by DIC. After humidity variations, the sample was analyzed by SEM to obtain the mineral map on the same surface to compare it with the location of desiccation cracks. 2 GEOLOGICAL SETTING AND SAMPLING The Tournemire Underground Laboratory (URL) of the French Institute for Radioprotection and Nuclear Safety (IRSN) is located in a Mesozoic marine basin on the southern limit of the Causse du Larzac. The sample used in this study is a cub of 20 × 20 × 20 mm3 extracted from the drill FD90 five meters deep in the East96 gallery. It comes from decimeter samples (d = 80 mm, L = 200 mm) between 4.20 and 4.40 meter, where the rock is considered as saturated and kept away outside from EDZ. The mineralogical composition of the rock shows that clay minerals represent about 20–50 wt% (kaolinite, illite, interstratified illite/smectite,), quartz about 10–20 wt %, carbonates about 10–30 wt% (calcite, dolomite, siderite), and sulphides 2–7 wt% (pyrites) (Cabrera et al. 2001). One face of the sample is finely polished to avoid topographic artefacts for SEM imaging and to have a good contrast for DIC. 1421 Figure 2. Extract from a DIC image (on the left) and the corresponding mineral map (on the right) for a region of interest. Figure 1. Experimental setup. Table 1. Humidity steps applied to the sample. 3 3.1 Desiccation 1 98 → 33% Hydration Desiccation 2 33 → 98% 98 → 33% EXPERIMENTAL SETUP AND METHODS Experimental setup physical transformation as mechanical or hydric loadings. The images are composed of pixels and each one is encoded by a grey level between 0 and 255 (8 bits). The method is based on the comparison of small domains (subsets) of grey levels between two images, in order to obtain the local displacement fields U which are estimated thanks to the positional changes of the grey level pattern in the subsets. The speckle pattern is usually artificial to have good variations of contrast but in this study, the speckle is the natural surface of the sample. The software used was XCorrel (H-DIC) developed by Pprime Institute of Poitiers (V. Valle et al. 2014). It allows the detection of displacement jumps which characterize the location of desiccation cracks on the sample surface. The domains are 32 × 32 pixels (70.4 × 70.4 µm2 ) with a precision of 0.1 pixel (0.22 µm). The experimental setup is composed of a plastic waterproof box in which humidity and temperature conditions are controlled. Relative humidity is controlled by saline solutions and temperature by an air-conditioning unit at 23◦ C. The box contains a RH/T (relative humidity/temperature) sensor, a precision balance and a stirred saline solution. The solution stirring is controlled by a programmable electric plug and imposed for 2 min over 15 min to preserve a constant temperature inside. A camera of 5 Mp (2560 × 1920 pixels) takes images (0.5image.min−1 ) with a spatial resolution of 2.2 µm.pixel−1 . A spot of 400 W lights up the sample while the camera taking an image. The sample was saturated for two months with a relative humidity of 98%. Then, it was submitted to a cycle of desiccation/hydration cycle between 98 and 33% of humidity during 55 days (Table 1). After the desiccation 2, the sample was analyzed under SEM with back-scattered electron to obtain the mineral map on the same surface. 3.2.2 Scanning Electron Microscopy (SEM) After the desiccation 2 (table 2), the surface which was recorded by DIC was analyzed under SEM with back-scattered electrons (BSE). This type of analysis is sensitive to the mean atomic number encoded by grey levels. A mineral map of the surface of 5.6 × 4.2 mm2 was investigated by acquiring a mosaic image of 8806 × 6606 pixels with a resolution of 0.625 µm.pixel−1 . The drift of the electron beam was estimated by measuring displacement, rotation, deformation and grey levels changes of BSE images. The displacement and the grey levels of the SEM images were corrected and the deformation and rotation were considered as insignificant. The precision of the superimposition between displacement fields from DIC and the SEM mosaic image is ±2 pixels (4.4 µm).The software µPHASEmap developed in IC2MP laboratory in Poitiers allows to threshold clay matrix and non-clay grains (Prêt et al. 2010 a,b) (Figure 2). 3.2 4 Methods 3.2.1 Digital Image Correlation (DIC) Optical full field measurement methods are more and more used in experimental mechanics. These techniques have many advantages like the non-destruction of the samples and the full-field data. DIC method was chosen in this study among these methods. It allows the measurement of displacement and strain fields, the detection of heterogeneities like cracks or strain gradients due to contrasts of different mechanical properties. It consists in recording images during a 4.1 RESULTS AND COMMENTS Cracking organization On the mineral map, there are many cracks corresponded to real desiccation cracks and cracks formed after or before the hydric loading. DIC method allows the selection of only working desiccation cracks during the experiment. The desiccation cracks of the sample are divided in two networks. By DIC mapping of local displacements between the initialstate and the final state of 1422 Figure 3. Ux and Uy displacement fieldsat the end of the desaturation 1. Figure 4. a) Uy displacement field at the end of desaturation 1; b) mineralogy map from SEM, corresponding to the black rectangle zone on figure 3. the sample, a first network (network I) of cracks is composed of three principal macrocracks in the same direction of bedding planes (Figure 3). There is no vertical macrocracks, in comparison with the gallery fractures (Hedan et al. 2012; 2014). The cracks I are continuous and spaced out of 1 mm. The second network (network II) is composed of microcracks between the macrocracks I at the interfaces of grain/grain, grain/clay matrix or in clay matrix (Figure 4). By BSE imaging, they seem to be discontinuous. These observations about the network II confirm previous works (Montes et al. 2004) on argillite samples from the Meuse Haute Marne Underground Research Laboratory (MHM-URL) in Eastern France obtain only at small scale by ESEM. 4.2 Relationships between macrocracks and microstructure So as to compare the crack location to the microstructure, some textural parameters were calculated from the mineral map, with the softwares ImageJ and Visual Studio C++ in same local subsets that DIC domains (70.4 × 70.4 µm2 ) used previously. The parameters are: the local proportion of grains Pg (example: Pg = 60%: there are 60 percent of nonclay grains in the domain), the local mean size of nonclay grains S (pixels), the local mean orientation of grains α (degrees), the local mean ratio length/width of grains L/h (≥1) and the local number of grains N. The textural parameters are presented as 2D maps, which are compared to the crack location from DIC (lines on figure 5). The local textural heterogeneities are surrounded on the maps. Figure 5. Superimposition between crack I location and textural parameter maps for Pg, S, α, L/h and N. The first results show that the location of cracks I is influenced by mineralogical heterogeneities especially by Pg and S. The cracks are located at the interfaces between a local heterogeneity and a more homogeneous zone (zones with Pg < 0.3 and S < 700 pixels, Figure 5). 1423 The sole parameters Pg and S do not explain the complete location of desiccation cracks. It is necessary to consider α, L/h and N to understand it. When all the parameters are combined on a same map, a close relationship between location crack and mineral heterogeneities is displayed. 5 ACKNOWLEDGMENTS The authors wish to thank especially Pascal Touvenet, Pascal Rogeon, Claude Laforest and FrédéricLimousin in ENSIP, and NEEDS (Nucléaire: Énergie, Environnement, Déchets, Société) project for supporting this research work. CONCLUSION REFERENCES The new experimental setup investigated in this study allowed the coupling between DIC and SEM methods in order to compare the location of desiccation cracks with the microstructure of the argillaceous rock of Tournemire at millimeter scale. The previous research works on the comparison between mineralogy and fracturing were generally done on small areas (<400 × 400 µm2 ), due to the classical field of view analyzed by SEM and ESEM. In this study, the comparison was done on a surface of 5.6 × 4.2 mm2 , nearly 20 times as much as wider than the previous areas with high resolution under SEM. During a dry/wet cycle, the desiccation cracks were organized in two networks at two different scales. The network I is composed of continuous macro-cracks in the same direction that bedding planes. The second network is composed of discontinuous microcracks at the interfaces grain/grain, grain/matrix or in the clay matrix, between macrocracks I. There is a close relationship between the location of desiccation cracks I and mineralogical heterogeneities, including local proportion of grains and clay matric or mean size of grains, which constitute local mechanical incompatibilities. The study of the desiccation cracking was completed at the meso-scale (millimeter scale) and that permits to shed light on the detection of local mineralogical heterogeneities which are very difficult to identify at microscale (micrometer scale) or global scale (meter scale) due to resolution limitations. At the end, one of the objectives of this current work is the comparison between the evolution of the aperture/closure of cracks I to the relative humidity during the hydric loading. This comparison should provide physical insights into the understanding of the transient desiccation cracking behaviour observed by DIC in the galleries at the Tournemire experimental station. (Hedanet al. 2014). 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