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):
[15506]
Open Access
Abstract: Determination of mineral texture and diagenetic features in mudstones is crucial to reveal the history of their pore systems and provides key information to predict their future sealing ability, reactivity and storage capacity for sequestered CO2, hydrogen storage or nuclear waste disposal. To understand the spatial transport and storage of fluids, it is necessary to map the distribution of minerals and fractures in three dimensions (3D). This study proposes a novel, multi-scale three-dimensional (3D) imaging method, i.e., a combination of synchrotron- sourced micro- x-ray tomography and lab- sourced nano-tomography, to investigate the sedimentology and diagenetic features of the Bowland Shale, one of the most volumetrically important mudstone-dominated systems in the UK. Diagenetic minerals have been identified and characterised, including pyrite, calcite, kaolinite, illite, chlorite, dolomite, ankerite and authigenic quartz (micro-sized quartz and quartz overgrowths). Multi-scale 3D images provide detailed information about dolomite-ankerite zonation and carbonate dissolution pores. These features cannot be observed or quantified by conventional 2D methods, and they have not been reported in this subject area before. Using these results, potential reactions during carbon storage and other subsurface storage applications are predicted.
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Apr 2023
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I12-JEEP: Joint Engineering, Environmental and Processing
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Open Access
Abstract: Deformation bands, or tabular zones of localised strain, are a common manifestation of deformation in upper crustal sedimentary rocks. Any mining or energy-related engineering applications must consider the possibility of reactivating these pre-existing failure planes because doing so can cause seismicity and compartmentalise the reservoir. However, there has only been a small amount of research done on laboratory-induced deformation in rocks with natural deformation features.
On a low porosity bioclastic calcarenite from the Cotiella Basin, Spanish Pyrenees, our current experimental work aims to capture, for the first time to our knowledge, the dominant failure mechanisms during the reactivation of natural deformation bands oriented at different angles to the principal stress direction. At the I12-JEEP beamline at the synchrotron facility of Diamond Light Source, UK, we carried out triaxial compression experiments using a modified version of the Mjolnir cell used by Cartwright-Taylor et al., (2022) to examine how these highly heterogeneous rocks respond to additional mechanical deformation. During the deformation experiments, 4D (time and space) x-ray tomography images (8 m voxel size resolution) were acquired. We tested confining pressures between 10 MPa and 30 MPa.
The mechanical data demonstrate that the existence of natural deformation features within the tested samples weakens the material. For instance, solid samples of the host rock subjected to the same confining pressures had higher peak differential stresses. Additionally, our findings demonstrate that new deformation bands form as their angle, θ, to σ1 increases, while the reactivation of pre-exiting deformation bands in this low porosity carbonate only occurs for dipping angles close to 70o. The spatio-temporal relationships between the naturally occurring and laboratory-induced deformation bands and fractures were investigated using time-resolved x-ray tomography and Digital Volume Correlation (DVC). Volumetric and shear strain fields were calculated using the SPAM software (Stamati et al., 2020). The orientation of the recently formed failure planes is influenced by the orientation of the pre-existing bands, as well as their width and the presence (or absence) of porosity along their length. Additionally, pre-existing secondary deformation features found in the tested material trigger additional mechanical damage that either promotes the development or deflects the new failure planes.
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Feb 2023
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[16205]
Open Access
Abstract: Methane (CH4) hydrate dissociation and CH4 release are potential geohazards currently investigated using X-ray computed tomography (XCT). Image segmentation is an important data processing step for this type of research. However, it is often time consuming, computing resource-intensive, operator-dependent, and tailored for each XCT dataset due to differences in greyscale contrast. In this paper, an investigation is carried out using U-Nets, a class of Convolutional Neural Network, to segment synchrotron XCT images of CH4-bearing sand during hydrate formation, and extract porosity and CH4 gas saturation. Three U-Net deployments previously untried for this task are assessed: (1) a bespoke 3D hierarchical method, (2) a 2D multi-label, multi-axis method and (3) RootPainter, a 2D U-Net application with interactive corrections. U-Nets are trained using small, targeted hand-annotated datasets to reduce operator time. It was found that the segmentation accuracy of all three methods surpass mainstream watershed and thresholding techniques. Accuracy slightly reduces in low-contrast data, which affects volume fraction measurements, but errors are small compared with gravimetric methods. Moreover, U-Net models trained on low-contrast images can be used to segment higher-contrast datasets, without further training. This demonstrates model portability, which can expedite the segmentation of large datasets over short timespans.
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Dec 2022
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I12-JEEP: Joint Engineering, Environmental and Processing
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Alexis
Cartwright-Taylor
,
Maria-Daphne
Mangriotis
,
Ian G.
Main
,
Ian B.
Butler
,
Florian
Fusseis
,
Martin
Ling
,
Edward
Andò
,
Andrew
Curtis
,
Andrew F.
Bell
,
Alyssa
Crippen
,
Roberto E.
Rizzo
,
Sina
Marti
,
Derek D. V.
Leung
,
Oxana V.
Magdysyuk
Diamond Proposal Number(s):
[22517]
Open Access
Abstract: Catastrophic failure in brittle, porous materials initiates when smaller-scale fractures localise along an emergent fault zone in a transition from stable crack growth to dynamic rupture. Due to the rapid nature of this critical transition, the precise micro-mechanisms involved are poorly understood and difficult to image directly. Here, we observe these micro-mechanisms directly by controlling the microcracking rate to slow down the transition in a unique rock deformation experiment that combines acoustic monitoring (sound) with contemporaneous in-situ x-ray imaging (vision) of the microstructure. We find seismic amplitude is not always correlated with local imaged strain; large local strain often occurs with small acoustic emissions, and vice versa. Local strain is predominantly aseismic, explained in part by grain/crack rotation along an emergent shear zone, and the shear fracture energy calculated from local dilation and shear strain on the fault is half of that inferred from the bulk deformation.
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Oct 2022
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[26232]
Abstract: Neutron and X-ray tomography (NCT and XCT, respectively) are imaging techniques increasingly being applied in geomechanics research. They are used to non-destructively reveal different microstructural aspects of geomaterials: XCT is often used to observe/quantify differences in density or porosity, while NCT reveals the presence and distribution of hydrogenous materials such as water. The correlated use of NCT and XCT for geomechanics and geotechnics research is in its infancy. To this date, very few experiments have been carried out that combine both techniques, and none have been used to investigate geomaterial-structure interaction. This paper presents the first correlative NCT-XCT imaging study of pile installation. A scaled model pile was installed in an unsaturated intact chalk cylinder and in-situ NCT and ex-situ XCT synchrotron-based imaging was applied consecutively. Chalk was used because the behaviour of displacement piles installed in this material is still subject to considerable uncertainty. Results reveal for the first time the interaction between installation-induced changes in chalk density and water distribution variations, with evidence of water displacement into the densified material in the vicinity of the installed pile. A straightforward method for correlative bulk density-moisture content determination from NCT-XCT images of geomaterials are presented and their limitations discussed.
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Jul 2022
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[16205]
Open Access
Abstract: Gas bubble in aquatic sediments has a significant effect on its geophysical and geomechanical properties. Recent studies have shown that methane gas and hydrate can coexist in gas hydrate–bearing sediments. Accurate calibration and understanding of the fundamental processes regarding such coexisting gas bubble dynamics is essential for geophysical characterization and hazard mitigation. We conducted high-resolution synchrotron imaging of methane hydrate formation from methane gas in water-saturated sand. While previous hydrate synchrotron imaging has focused on hydrate evolution, here we focus on the gas bubble dynamics. We used a novel semantic segmentation technique based on convolutional neural networks to observe bubble dynamics before and during hydrate formation. Our results show that bubbles change shape and size even before hydrate formation. Hydrate forms on the outer surface of the bubbles, leading to reduction in bubble size, connectivity of bubbles, and the development of nano-to micro-sized bubbles. Interestingly, methane gas bubble size does not monotonously decrease with hydrate formation; rather, we observe some bubbles being completely used up during hydrate formation, while bubbles originate from hydrates in other parts. This indicates the dynamic nature of gas and hydrate formation. We also used an effective medium model including gas bubble resonance effects to study how these bubble sizes affect the geophysical properties. Gas bubble resonance modeling for field or experimental data generally considers an average or equivalent bubble size. We use synchrotron imaging data to extract individual gas bubble volumes and equivalent spherical radii from the segmented images and implement this into the rock physics model. Our modeling results show that using actual bubble size distribution has a different effect on the geophysical properties compared to the using mean and median bubble size distributions. Our imaging and modeling studies show that the existence of these small gas bubbles of a specific size range, compared to a bigger bubble of equivalent volume, may give rise to significant uncertainties in the geophysical inversion of gas quantification.
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Jun 2022
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[26307]
Open Access
Abstract: X-ray computed tomography (XCT) is regularly employed in geomechanics to non-destructively measure the solid and pore fractions of soil and rock from reconstructed 3D images. With the increasing availability of high-resolution XCT imaging systems, researchers now seek to measure microfabric parameters such as the number and area of interparticle contacts, which can then be used to inform soil behaviour modelling techniques. However, recent research has evidenced that conventional image processing methods consistently overestimate the number and area of interparticle contacts, mainly due to acquisition-driven image artefacts. The present study seeks to address this issue by systematically assessing the role of XCT acquisition parameters in the accurate detection of interparticle contacts. To this end, synchrotron XCT has been applied to a hexagonal close-packed arrangement of glass pellets with and without a prescribed separation between lattice layers. Different values for the number of projections, exposure time, and rotation range have been evaluated. Conventional global grey value thresholding and novel U-Net segmentation methods have been assessed, followed by local refinements at the presumptive contacts, as per recently proposed contact detection routines. The effect of the different acquisition set-ups and segmentation techniques on contact detection performance is presented and discussed, and optimised workflows are proposed.
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May 2022
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[18758]
Abstract: Natural surface gas seeps provide a significant input of greenhouse gas emissions into the Earth’s atmosphere and hydrosphere. The gas flux is controlled by the properties of underlying fluid-escape conduits, which are present within sedimentary basins globally. These conduits permit pressure-driven fluid flow, hydraulically connecting deeper strata with the Earth’s surface; however they can only be fully resolved at sub-seismic scale. Here, a novel ‘minus cement and matrix permeability’ method using three-dimensional X-ray micro-computed tomography imaging enables the improved petrophysical linkage of outcrop and sub-surface data. The methodology is applied to the largest known outcrop of an inactive fluid-escape system, the Panoche Giant Intrusion Complex in Central California, where samples were collected along transects of the 600 to 800 m stratigraphic depth range to constrain porosity and permeability spatial heterogeneity. The presence of silica cement and clay matrix within the intergranular pores of sand intrusions are the primary control of porosity (17 to 27%) and permeability (≤1 to ca 500 mD) spatial heterogeneity within the outcrop analogue system. Following the digital removal of clay matrix and silica (opal-CT and quartz) cement derived from the mudstone host strata, the sand intrusions have porosity-permeability ranges of ca 30 to 40% and 103 to 104 mD. These calculations are closely comparable to active sub-surface systems in sedimentary basins. Field observations revealed at decreasing depth, the connected sand intrusion network reduces in thickness and becomes carbonate cemented, terminating at carbonate mounds formed from methane escape at the seafloor. A new conceptual model integrates the pore-scale calculations and field-scale observations to highlight the key processes that control sand intrusion permeability, spatially and temporally. The study demonstrates the control of matrix and cement addition on the physical properties of fluid-escape conduits, which has significance for hydrocarbon reservoir characterization and modelling, as well as subsurface CO2 and energy storage containment assessment.
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Apr 2022
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I12-JEEP: Joint Engineering, Environmental and Processing
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Abstract: Zero carbon energy generation from renewable sources can reduce climate change by mitigating carbon emissions. A major challenge of renewable energy generation is the imbalance between supply and demand. To overcome the energy imbalances, subsurface storage of hydrogen in porous mediais suggested as a large-scale and economic solution, yet its mechanisms are not fully understood. Important unknowns are the effect of the high migration potential of the small and mobile hydrogen molecule and the volume of recoverable hydrogen.
We conducted non-steady state, cyclic hydrogen and brine injection experiments at 2-7 MPa and flow rates of 2-80 µl min-1 using water-wet Clashach sandstone cylinders of 4.7 mm diameter and 53-57 mm length (Clashach composition: ~96 wt.% quartz, 2% K-feldspar, 1% calcite, 1% ankerite). Two sets of experiments were performed using our new transparent flow-cell designed for x-ray computed microtomography: 1) Experiments using a laboratory x-ray source (University of Edinburgh) imaged the flow, displacement and capillary trapping of hydrogen by brine as a function of saturation after primary drainage and secondary imbibition. 2) Experiments using synchrotron radiation (Diamond Light Source, I12-JEEP tomography beamline) captured time-resolved hydrogen and brine flow and displacement processes. Pressure and mass flow measurements across the experimental apparatus complemented the microtomography volumes in both sets of experiments.
Results from a water-wet rock show that hydrogen behaves as a non-wetting phase and sits in the centre of the pore bodies, while residual brine sits in corners and pore throats. Hydrogen saturation in the pore volume is independent of the injection pressure and increases with increasing hydrogen/brine injection ratio up to ~50% saturation at 100 % hydrogen. Capillary trapping of hydrogen during brine imbibition occurs via snap off and is greatest at higher brine injection pressures, with 10 %, 12% and 21% hydrogen trapped at 2, 5 and 7 MPa, respectively. Higher brine flow rates reduce capillary trapping and increase hydrogen recovery at any given injection pressure. Based on these results, future hydrogen storage operations should inject 100% hydrogen and manage the reservoir pressure to avoid high pressures and minimize capillary trapping of hydrogen during brine reinjection.
Ongoing analysis of time-resolved experimental data will provide further insight into the critical pore-scale processes that ultimately influence the potential for geological hydrogen storage and recovery.
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Mar 2022
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