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The input sediments of the North Sumatra subduction zone margin, drilled during IODP Expedition 362, exhibit remarkable uniformity in composition and grain size over the entire thickness of the rapidly deposited Nicobar Fan succession (seafloor to 1500 m b.s.f.), providing a unique opportunity to study the micromechanisms of compaction. Samples were prepared from dried core samples (from Sites U1480 and U1481) by both Ar-ion cross-section polishing and broad ion beam cutting and imaged with a field-emission scanning electron microscope (SEM). The shallowest samples (seafloor to 28 m b.s.f.) display a sharp reduction in porosity from 80 % to 52 % due to collapse of large clay-domain surrounding matrix pores associated with rotation and realignment of clay platelets parallel to the bedding plane. The deeper succession (28 to 1500 m b.s.f.) exhibits less rapid reduction in porosity from 52 % to 30 % by the progressive collapse of silt-adjacent larger pores through bending as well as subsequent sliding and/or fracturing of clay particles. In addition, there is a correlated loss of porosity in the pores too small to be resolved by SEM. Clastic particles show no evidence of deformation or fracturing with increasing compaction. In the phyllosilicates, there is no evidence for pressure solution or recrystallization: thus, compaction proceeds by micromechanical processes. An increase in effective stress up to 18 MPa (∼ 1500 m b.s.f.) causes the development of a weakly aligned phyllosilicate fabric mainly defined by illite clay particles and mica grains, while the roundness of inter-particle pores decreases as the pores become more elongated. We propose that bending of the phyllosilicates by inter-particle slip may be the rate-controlling mechanism. Pore size distributions show that all pores within the compactional force chain deform, irrespective of size, with increasing compactional strain. This arises because the force chain driving pore collapse is localized primarily within the volumetrically dominant and weaker clay-rich domains; pores associated with packing around isolated silt particles enter into the force chain asynchronously and do not contribute preferentially to pore loss over the depth range studied.

A microphysics-based understanding of mechanical and hydraulic processes in clay shales is required for developing advanced constitutive models, which can be extrapolated to long-term deformation. Although many geomechanical tests have been performed to characterise the bulk mechanical, hydro-mechanical, and failure behaviour of Opalinus Clay, important questions remain about micromechanisms: how do microstructural evolution and deformation mechanisms control the complex rheology? What is the in situ microstructural shear evolution, and can it be mimicked in the laboratory? In this contribution, scanning electron microscopy (SEM) was used to image microstructures in an Opalinus Clay sample deformed in an unconsolidated–undrained triaxial compression test at 4 MPa confining stress followed by argon broad ion beam (BIB) polishing. Axial load was applied (sub-)perpendicular to bedding until the sample failed. The test was terminated at an axial strain of 1.35 %. Volumetric strain measurements showed bulk compaction throughout the compression test. Observations on the centimetre to micrometre scale showed that the samples exhibited shear failure and that deformation localised by forming a network of micrometre-wide fractures, which are oriented with angles of 50∘ with respect to horizontal. In BIB–SEM at the grain scale, macroscale fractures are shown to be incipient shear bands, which show dilatant intergranular and intragranular microfracturing, granular flow, bending of phyllosilicate grains, and pore collapse in fossils. Outside these zones, no deformation microstructures were observed, indicating only localised permanent deformation. Thus, micromechanisms of deformation appear to be controlled by both brittle and ductile processes along preferred deformation bands. Anastomosing networks of fractures develop into the main deformation bands with widths up to tens of micrometres along which the sample fails. Microstructural observations and the stress–strain behaviour were integrated into a deformation model with three different stages of damage accumulation representative for the deformation of the compressed Opalinus Clay sample. Results on the microscale explain how the sample locally dilates, while bulk measurement shows compaction, with an inferred major effect on permeability by an increase in hydraulic conductivity within the deformation band. Comparison with the microstructure of highly strained Opalinus Clay in fault zones shows partial similarity and suggests that during long-term deformation additional solution–precipitation processes operate.

Estimating the porosity of slates is of great interest for the industries dealing with sub-surface areas such as CO2 sequestration, nuclear waste disposal and shale gas but also for engineering purposes in terms of mechanical stability for underground or surface constructions. In this study, we aim at understanding estimates of the porosity of slates from the Infrahelvetic flysch units (IFUs) in the Glarus Alps (eastern Switzerland). Surface and sub-surface samples were collected along a temperature gradient from 200 to 320 °C and therefore give the opportunity to link pore types along this temperature and deformation path. In addition, we indicate which porosity is the effect of surface processes and indicate the contribution of artificially induced porosity. The developed workflow consists of a combination of bulk rock measurements including helium pycnometry (He pycnometry) and mercury intrusion porosimetry (MIP) with image analysis. Image analysis was performed with high-resolution scanning electron microscopy (SEM) on broad ion beam (BIB) prepared cross sections (BIB-SEM). Different vein generations provide evidence of porosity formation at depth, as they present paleo-porosity. Towards peak metamorphic conditions (prograde path), porosity reduces to

The macroscopic description of deformation and fluid flow in mudrocks can be improved by a better understanding of microphysical deformation mechanisms. Here we use a combination of scanning electron microscopy (SEM) and broad ion beam (BIB) polishing to study the evolution of microstructure in samples of triaxially deformed Callovo–Oxfordian Clay. Digital image correlation (DIC) was used to measure strain field in the samples and as a guide to select regions of interest in the sample for BIB–SEM analysis. Microstructures show evidence for dominantly cataclastic and minor crystal plastic mechanisms (intergranular, transgranular, intragranular cracking, grain rotation, clay particle bending) down to the nanometre scale. At low strain, the dilatant fabric contains individually recognisable open fractures, while at high strain the reworked clay gouge also contains broken non-clay grains and smaller pores than the undeformed material, resealing the initial fracture porosity.

Microstructure strongly influences flow and transport properties of porous media. Flow and transport simulations within porous media, therefore, requires accurate three-dimensional (3D) models of the pore and solid phase structure. To date, no imaging method can resolve all relevant heterogeneities from the nano- to the centimeter scale within complex heterogeneous materials such as clay, reservoir rocks (e.g., travertine, chalk, ...), hardened cement paste, and concrete. To reconstruct these porous materials it is thus necessary to merge information from different 2D and potentially 3D imaging methods. One porous media reconstruction methodology that has been around for at least two decades is simulated annealing (SA). However, realizations with SA typically suffer an artificially reduced long-range connectivity, while multiphase reconstructions are not feasible in most cases because of a prohibitive computational burden. To solve these problems we propose a hierarchical multiresolution and multiphase simulated annealing algorithm. To decrease the computational cost of multiphase simulation, our algorithm sequentially simulates one phase after another, in a hierarchical way, which enables handling multimodal distributions and topological relations. Building upon recent work, our algorithm improves long-range connectivity and CPU efficiency by simulating larger particles using a coarser resolution that is subsequently refined compared to standard SA; our proposed extension not only offers the possibility to perform multiphase reconstruction but also allows us (i) to improve binary reconstruction quality, as quantified, e.g., by multiple-point histograms by up to one order of magnitude and (ii) to achieve an overall speed-up. The proposed algorithm is also shown to outperform the direct sampling multiple-point statistics method for the generation of cement paste microstructure with respect to both generation time and quality.

The contribution describes the implementation of a broad ion beam (BIB) polisher into a scanning electron microscope (SEM) functioning at cryogenic temperature (cryo). The whole system (BIB-cryo-SEM) provides a first generation of a novel multibeam electron microscope that combines broad ion beam with cryogenic facilities in a conventional SEM to produce large, high-quality cross-sections (up to 2 mm(2)) at cryogenic temperature to be imaged at the state-of-the-art SEM resolution. Cryogenic method allows detecting fluids in their natural environment and preserves samples against desiccation and dehydration, which may damage natural microstructures. The investigation of microstructures in the third dimension is enabled by serial cross-sectioning, providing broad ion beam tomography with slices down to 350 nm thick. The functionalities of the BIB-cryo-SEM are demonstrated by the investigation of rock salts (synthetic coarse-grained sodium chloride synthesized from halite-brine mush cold pressed at 150 MPa and 4.5 GPa, and natural rock salt mylonite from a salt glacier at Qom Kuh, central Iran). In addition, results from BIB-cryo-SEM on a gas shale and Boom Clay are also presented to show that the instrument is suitable for a large range of sedimentary rocks. For the first time, pore and grain fabrics of preserved host and reservoir rocks can be investigated at nm-scale range over a representative elementary area. In comparison with the complementary and overlapping performances of the BIB-SEM method with focused ion beam-SEM and X-ray tomography methods, the BIB cross-sectioning enables detailed insights about morphologies of pores at greater resolution than X-ray tomography and allows the production of large representative surfaces suitable for FIB-SEM investigations of a specific representative site within the BIB cross-section., (© 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.)

Examination of very long hair (length > 2.4 m) using a large range of evaluation methods including physical, chemical, biochemical and microscopic techniques has enabled to attain a detailed understanding of natural ageing of human hair keratin fibres. Scrutinizing hair that has undergone little or no oxidative aggression--because of the absence of action of chemical agents such as bleaching or dyeing--from the root to the tip shows the deterioration process, which gradually takes place from the outside to the inside of the hair shaft: first, a progressive abrasion of the cuticle, whilst the cortex structure remains unaltered, is evidenced along a length of roughly 1 m onwards together with constant shine, hydrophobicity and friction characteristics. Further along the fibre, a significant damage to cuticle scales occurs, which correlates well with ceramides and 18-Methyl Eicosanoic Acid (18-MEA) decline, and progressive decrease in keratin-associated protein content. Most physical descriptors of mechanical and optical properties decay significantly. This detailed description of natural ageing of human hair fibres by a fine analysis of hair components and physical parameters in relationship with cosmetic characteristics provides a time-dependent 'damage scale' of human hair, which may help in designing new targeted hair care formulations.