I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[28557]
Open Access
Abstract: Swelling of shale in response to interaction with water is an important consideration within subsurface energy systems. In the case of waste disposal, swelling can provide important barriers around the waste and enhance the sealing ability of rocks. For shale gas exploration purpose, however, swelling may cause wellbore instability. Therefore, a careful study of shale swelling is critical for subsurface energy related applications. Here, the swelling effects of shale were imaged at nanoscale using an advanced synchrotron Transmission X-ray Microscopy (TXM) imaging technique for the first time, with a spatial resolution down to 40.9 nm. Organic matter and clays within the analysed sample were observed to display large swelling effects which resulted in a 50% reduction in porosity. Strain maps generated using Digital Volume Correlation (DVC) show deformation and significant strain were mostly localized to between the contact boundaries of sharp brittle minerals and softer organic matter and clays. This is the first study, to our knowledge, to directly image the swelling deformation of shale at the tens of nanometer scale and provide local information on the strain evolution.
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Jul 2023
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[19904]
Open Access
Abstract: The development of pore and fracture networks at the nano-scale as a response to heating can reveal coupled physical relationships relevant to several energy applications. A combination of time-lapse 3D imaging and finite-element modelling (FEM) was performed on two typical thermally immature shale samples, Kimmeridge Clay and Akrabou shale, to investigate thermal response at the nm-scale for the first time. Samples were imaged using Transmission X-ray Microscopy (TXM) with a voxel resolution of 34 nm at the I13–2 beamline at Diamond Light source, UK. Images were taken after heating to temperatures of 20 °C, 300 °C, 350 °C and 400 °C. The initiation of nano-pores within individual minerals and organic matter particles were observed and quantified alongside the evolution from nano-pores to micro-fractures. The major expansion of pore-volume occurred between 300 and 350 °C in both samples, with the pores elongating rapidly along the organic-rich bedding. The internal pressures induced by organic matter transformation influenced the development of microfractures. Mechanical properties and strain distributions within these two samples were modelled under a range of axial stresses using FEM. The results show that the overall stiffness of the shale reduced during heating, despite organic matter becoming stiffer. The varied roles of ductile (e.g., clay minerals, organic matter) and brittle materials (e.g., calcite, pyrite) within the rock matrix are also modelled and discussed. The configurations of organic matter, mineral components, porosity and connectivity impact elastic deformation during shale pyrolysis. This work extends our understanding of dynamic coupled processes of microstructure and elastic deformation in shales to the nm-scale, which also has applications to other subsurface energy systems such as carbon sequestration, geothermal and nuclear waste disposal.
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Jun 2021
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I12-JEEP: Joint Engineering, Environmental and Processing
I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[13824, 9866, 17606]
Open Access
Abstract: Injection of CO2 into shale reservoirs to enhance gas recovery and simultaneously sequester greenhouse gases is a potential contributor towards the carbon-neutral target. It offers a low-carbon, low-cost, low-waste and large-scale solution during the energy transition period. A precondition to efficient gas storage and flow is a sound understanding of how the shale's micro-scale impacts on these phenomena. However, the heterogeneous and complex nature of shales limits the understanding of microstructure and pore systems, making feasibility analysis challenging. This study qualitatively and quantitatively investigates the Bowland shale microstructure in 3D at five length scales: artificial fractures at 10–100 μm scale, matrix fabric at 1–10 μm-scale, individual mineral grains and organic matter particles at 100 nm–1 μm scale, macropores and micro-cracks at 10–100 nm scale and organic matter and mineral pores at 1–10 nm-scale. For each feature, the volume fraction variations along the bedding normal orientation, the fractal dimensions and the degrees of anisotropy were analysed at all corresponding scales for a multi-scale heterogeneity analysis. The results are combined with other bulk laboratory measurements, including supercritical CO2 and CH4 adsorption at reservoir conditions, pressure-dependent permeability and nitrogen adsorption pore size distribution, to perform a comprehensive analysis on the storage space and flow pathways. A cross-scale pore size distribution, ranging from 2 nm to 3 μm, was calculated with quantified microstructure. The cumulative porosity is calculated to be 8%. The cumulative surface area is 17.6 m2 g−1. A model of CH4 and CO2 flow pathways and storage with quantified microstructure is presented and discussed. The feasibility of simultaneously enhanced gas recovery and subsurface CO2 storage in Bowland shale, the largest shale gas potential formation in the UK, was assessed based using multi-scale microstructure analysis. The potential is estimated to store 19.0–21.2 Gt CO2 as free molecules, together with 18.3–28.5 Gt CO2 adsorbed onto pore surfaces, implying a theoretical maximum of 47.5–49.5 Gt carbon storage in the current estimate of 38 trillion cubic metres (∼1300 trillion cubic feet) of Bowland shale. Simple estimates suggest 6.0–15.8 Gt CO2 may be stored in practice.
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Jun 2021
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[15506]
Abstract: The feasibility and advantages of synchrotron imaging have been demonstrated to effectively characterise fracture initiation and propagation in shales during indentation tests. These include 1) fast (minute-scale) and high-resolution (μm-scale) imaging of fracture initiation, 2) concurrent spatial and temporal information (4D) about fracture development, 3) quantification and modelling of shale deformation prior to fracture. Imaging experiments were performed on four shale samples with different laminations and compositions in different orientations, representative of three key variables in shale microstructure. Fracture initiation and propagation were successfully captured in 3D over time, and strain maps were generated using digital volume correlation (DVC). Subsequently, post-experimental fracture geometries were characterized at nano-scale using complementary SEM imaging. Characterisation results highlight the influence of microstructural and anisotropy variations on the mechanical properties of shales. The fractures tend to kink at the interface of two different textures at both macroscale and microscale due to deformation incompatibility. The average composition appears to provide the major control on hardness and fracture initiation load; while the material texture and the orientation of the indentation to bedding combine to control the fracture propagation direction and geometry. This improved understanding of fracture development in shales is potentially significant in the clean energy applications.
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Oct 2020
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[17314]
Open Access
Abstract: Barite precipitation in fractures and nanopores within a shale sample is analysed in situ, in 3D, and over time. Diffusion of barium and sulphate from opposite sides of the sample creates a supersaturated zone where barium sulphate crystals precipitate. Time-lapse synchrotron-based computed tomography was used to track the growth of precipitates over time, even within the shale’s matrix where the nanopores are much smaller than the resolution of the technique. We observed that the kinetics of precipitation is limited by the type and size of the confinement where crystals are growing, i.e., nanopores and fractures. This has a major impact on the ion transport at the growth front, which determines the extent of precipitation within wider fractures (fast and localised precipitation), thinner fractures (non-localised and slowing precipitation) and nanopores (precipitation spread as a front moving at an approximately constant velocity of 10 ± 3 µm/h). A general sequence of events during precipitation in rocks containing pores and fractures of different sizes is proposed and its possible implications to earth sciences and subsurface engineering, e.g., fracking and mineral sequestration, are discussed.
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Aug 2019
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[4022]
Abstract: Microstructures and pore systems in shales are key to understanding the role of shale in many energy applications. This study proposes a novel multi-stage upscaling procedure to comprehensively investigate the heterogeneous and complex microstructures and pore systems in a laminated and microfractured shale, utilizing 3D multi-scale imaging data. Five imaging techniques were used for characterisation from sub-nanoscale to macroscale (core-scale), spanning four orders of magnitude. Image data collected using X-ray tomography, Focused Ion Beam, and Electron Tomography techniques range in voxel size from 0.6 nm to 13 μm.
Prior to upscaling, a novel two-step analysis was performed to ensure sub-samples were representative. Following this, a three-step procedure, based on homogenising descriptors and computed volume coefficients, was used to upscale the quantified microstructure and pore system. At the highest resolution (nanoscale), four distinct pore types were identified. At the sub-micron scale equations were derived for three pore-associated phases. At the microscale, the volume coefficients were recalculated to upscale the pore system to the macroscale (millimetre). The accuracy of the upscaling methodology was verified, predicting the total porosity within 7.2% discrepancy. The results provide a unique perspective to understand heterogeneous rock types, breaking though prior scale limitations in the pore system.
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Jun 2019
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I12-JEEP: Joint Engineering, Environmental and Processing
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Michael R.
Chandler
,
Anne-Laure
Fauchille
,
Ho Kyeom
Kim
,
Lin
Ma
,
Julian
Mecklenburgh
,
Roberto
Rizzo
,
Mahmoud
Mostafavi
,
Sebastian
Marussi
,
Robert
Atwood
,
Steven
May
,
Mohammed
Azeem
,
Ernie
Rutter
,
Kevin
Taylor
,
Peter
Lee
Diamond Proposal Number(s):
[13824]
Open Access
Abstract: Mode‐I Fracture Toughness, KIc, was measured in six shale materials using the double torsion technique. During loading, crack propagation was imaged both using twin optical cameras, and with fast X‐Ray radiograph acquisition. Samples of Bowland, Haynesville, Kimmeridge, Mancos, Middlecliff and Whitby shales were tested in a range of orientations. The measured fracture toughness values were found to be in good agreement with existing literature values. The two imaging techniques improve our understanding of local conditions around the fracture tip, through in‐situ correlation of mechanical data, inelastic zone size and fracture‐tip velocity. The optical Digital Image Correlation (DIC) technique proved useful as a means of determining the validity of individual experiments, by identifying experiments during which strains had developed in the two "rigid" specimen halves. Strain maps determined through DIC of the optical images suggest that the scale of the inelastic zone is an order of magnitude smaller than the classically used approximation suggests. This smaller damage region suggests a narrower region of enhanced permeability around artificially generated fractures in shales. The resolvable crack‐tip was tracked using radiograph data and found to travel at a velocity around 470μm.s−1 during failure, with little variation in speed between materials and orientations. Fracture pathways in the bedding parallel orientations were observed to deviate from linearity, commonly following layer boundaries. This suggests that while a fracture travelling parallel to bedding may travel at a similar speed to a bedding perpendicular fracture, it may have a more tortuous pathway, and therefore access a larger surface area.
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Dec 2018
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[4022]
Open Access
Abstract: Understanding the distribution of pores and organic matter with varying organic matter concentrations and maturity is essential to understanding fluid flow in shale systems. Analysis of samples with low, medium, and high total organic carbon (TOC) and varying maturities (gas-mature and oil-mature) enables the impact of both organic matter concentrations and thermal maturation on organic matter porosity to be examined. Three gas-mature samples of varying TOC (Lublin Basin) and one oil-mature sample (Baltic Basin), both with similar mineral compositions, were selected from the same formation. Samples were imaged in 3D over four orders of magnitudes (pixel sizes from 44 μm to 5 nm). A combination of X-ray computed tomography (XCT) and Focus Ion Beam Scanning Electron Microscopy (FIB-SEM) enabled the morphologic and topological characteristics of minerals, organic matter and pores to be imaged and quantified.
In the studied samples, organic matter primarily has two geometries: lamellar masses (length: 1–100 μm, thickness: 0.5–2.0 μm) and discrete spheroidal particles (0.5–20.0 μm). Organic matter forms an inter-connected network where it exceeds a concentration between 6 and 18 wt%.
Different pore types have different diameters and total pore volumes: inter-mineral pores (0.2 μm, 10–94%), organic interface pores (0.2 μm, 2–77%), intra-organic pores (0.05 μm, 1–40%) and intra-mineral pores (0.05 μm diameter, 1–2% of total porosity). The major pore system in the studied shales is composed of inter-mineral pores which occur between clay mineral grains. TOC concentration influences the total volume of organic matter-related pores while maturity controls the presence of intra-organic pores. The study improves the understanding of the relationship of organic matter concentrations, maturity and pore systems in shales. This study characterises porosity and organic matter distributions in 3D; it also improves the understanding of the relationship of organic matter concentrations, maturity and pore systems in shales.
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Aug 2017
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[9866]
Abstract: Analyzing the development of fracture networks in shale is important to understand both hydrocarbon migration pathways within and from source rocks, and the effectiveness of hydraulic stimulation upon shale reservoirs. Here we use time resolved synchrotron X-ray tomography to quantify in four dimensions (3D plus time) the development of fractures during the accelerated maturation of an organic-rich mudstone (the UK Kimmeridge Clay), with the aim of determining the nature and timing of crack initiation. Electron microscopy (EM, both scanning backscattered and energy dispersive) was used to correlatively characterize the microstructure of the sample pre- and post-heating. The tomographic data was analyzed using digital volume correlation (DVC) to measure the three-dimensional displacements between subsequent time/heating steps allowing the strain fields surrounding each crack to be calculated, enabling crack opening modes to be determined. Quantification of the strain eigenvectors just before crack propagation suggests the main mode driving crack initiation is the opening displacement perpendicular to the bedding, mode I. Further, detailed investigation of the DVC measured strain evolution revealed the complex interaction of the laminar clay matrix and the maximum principal strain on incipient crack nucleation. Full field DVC also allowed accurate calculation of the coefficients of thermal expansion (8x10-5/°C perpendicular, and 6.2x10-5/°C parallel to the bedding plane). These results demonstrate how correlative imaging (using synchrotron tomography, DVC, and EM) can be used to elucidate the influence of shale microstructure on its anisotropic mechanical behavior.
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Mar 2017
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I13-2-Diamond Manchester Imaging
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Open Access
Abstract: X-ray computed tomography and serial block face scanning electron microscopy imaging techniques were used to produce 3D images with a resolution spanning three orders of magnitude from ∼7.7 μm to 7 nm for one typical Bowland Shale sample from Northern England, identified as the largest potential shale gas reservoir in the UK. These images were used to quantitatively assess the size, geometry and connectivity of pores and organic matter. The data revealed four types of porosity: intra-organic pores, organic interface pores, intra- and inter-mineral pores. Pore sizes are bimodal, with peaks at 0.2 μm and 0.04 μm corresponding to pores located at organic–mineral interfaces and within organic matter, respectively. These pore-size distributions were validated by nitrogen adsorption data. The multi-scale imaging of the four pore types shows that there is no connected visible porosity at these scales with equivalent diameter of 20 nm or larger in this sample. However, organic matter and clay minerals are connected and so the meso porosity (<20 nm) within these phases provides possible diffusion transport pathways for gas. This work confirms multi-scale 3D imaging as a powerful quantification method for shale reservoir characterisation allowing the representative volumes of pores, organic and mineral phases to be defined to model shale systems. The absence of connected porosity at scales greater than 20 nm indicates the likely importance of the organic matter network, and associated smaller-scale pores, in controlling hydrocarbon transport. . The application of these techniques to shale gas plays more widely should lead to a greater understanding of properties in the low permeability systems.
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Apr 2016
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