I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[30455]
Open Access
Abstract: Permeability is a key rock property important for scientific applications that require simulation of fluid flow. Although permeability is determined using core flooding experiments, recent advancements in micro-CT imaging and pore scale fluid flow simulations have made it possible to constrain permeability honoring pore scale rock structure. Previous studies have reported that complex association of pores and solid grains often results in preferential flow paths which influence the resulting velocity field and, hence, the upscaled permeability value. Additionally, the pore structure may change due to geochemical processes such as microbial growth, mineral precipitation and dissolution. This could result in a flow field which dynamically evolves spatially and temporally. It would require numerous experiments or full physics simulations to determine the resultant upscaled Darcy permeability for such dynamically changing systems. This study presents a graph theory-based approach to upscale permeability from pore-to-Darcy scale for changing pore structure. The method involves transforming a given micro-CT rock image to a graph network map followed by the identification of the least resistance path between the inlet and the outlet faces using Dijkstra's algorithm where resistance is quantified as a function of pore sizes. The least resistance path is equivalent to the path of lowest resistance within the domain. The method was tested on micro-CT images of the samples of Sherwood Sandstone, Ketton Limestone and Estaillades Limestone. The three micro-CT images were used to generate 30 synthetic scenarios for geochemically induced pore structure changes covering a range of pore and solid grain growth. The least resistance value obtained from Dijkstra's algorithm was observed to correlate with upscaled permeability value determined from full physics simulations, while improving computational efficiency by a factor of 250. This provides confidence in using graph theory method as a proxy for full physics simulations for determining effective permeability for samples with changing pore structure.
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Sep 2024
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I13-2-Diamond Manchester Imaging
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Open Access
Abstract: This study extensively investigates the influence of different pyrolysis temperatures and organic matter contents on the fluid flow and heat transfer properties in oil shale samples. Utilizing CT images to generate three-dimensional digital rock, coupled simulations of CO2 flow and heat transfer were conducted, analyzing parameters such as velocity fields, permeability, temperature fields, average temperatures, and heat transfer coefficients. The results reveal that, for relatively homogeneous oil shale samples, the permeability exhibits a monotonous increase with rising pyrolysis temperature. While the effect of pyrolysis temperature on the distribution characteristics of velocity and temperature fields is minimal, it significantly impacts the heat transfer coefficients. Specifically, the heat transfer coefficients increase significantly in the direction perpendicular to the bedding plane, while they decrease or remain unchanged parallel to it. Additionally, the organic matter content significantly influences the fluid flow and heat transfer properties of shale samples. After undergoing heat treatment, the heterogeneity of pore structures in shale samples varies significantly, affecting the characteristics of fluid flow and heat transfer. The influence of organic matter content and pyrolysis temperature on fluid flow and heat transfer in shale primarily stems from the effect of organic matter pyrolysis on the original pore structure. The development and connectivity of pore networks are closely related to the distribution characteristics of the original organic matter and are not directly correlated with the organic matter content. These findings provide essential theoretical guidance and technical support for the development and utilization of oil shale resources, while also offering valuable references and insights for future research.
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Aug 2024
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I19-Small Molecule Single Crystal Diffraction
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Open Access
Abstract: The Earth can be viewed as a one-dimensional, layered, chemically differentiated planet, composed of crust, mantle, and core. These layers, and sub-layers within them, are separated by boundaries. Seismic tomography is the primary source for this information showing a change in chemistry and/or of crystal structure by locating and mapping reflections, refractions, and conversions of seismic waves along these boundaries. To understand the behaviour of the Earth’s upper mantle and mantle transition zone, the convection mechanisms, thermal properties, rheology, and to create accurate mineralogical models that reflect these properties, requires investigation of their constituent mineral phases. Most researchers tend to focus on the olivine content of the mantle, this being the most common mineral up to 660 km, underestimating the contribution of garnets and pyroxenes. This has led to gaps in the published literature with many garnet and pyroxene phases being very poorly constrained and, in some cases, not even explored. But even for olivines, there are properties that have not yet been determined. The aim of this PhD thesis is to fill some of these gaps and to provide new information for phases within the olivine, garnet, and pyroxene mineral groups. Both polycrystalline and single-crystal samples were synthesised using the multi-anvil press at UCL. After structure characterisation using X-ray diffraction at ambient conditions, all samples were analysed with either low/high-temperature or high-pressure Xray and neutron diffraction methods at university-based and synchrotron radiation facilities.
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Jul 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Simon A.
Hunt
,
Andrew M.
Walker
,
Oliver T.
Lord
,
Stephen
Stackhouse
,
Lewis
Schardong
,
Lora S.
Armstrong
,
Andrew J.
Parsons
,
Geoffrey E.
Lloyd
,
John
Wheeler
,
Danielle M.
Fenech
,
Stefan
Michalik
,
Matthew L.
Whitaker
Diamond Proposal Number(s):
[23970]
Open Access
Abstract: Seismic observations show the Earth's inner core has significant and unexplained variation in seismic attenuation with position, depth and direction. Interpreting these observations is difficult without knowledge of the visco- or anelastic dissipation processes active in iron under inner core conditions. Here, a previously unconsidered attenuation mechanism is observed in zinc, a low pressure analog of hcp-iron, during small strain sinusoidal deformation experiments. The experiments were performed in a deformation-DIA combined with X-radiography, at seismic frequencies (∼0.003–0.1 Hz), high pressure and temperatures up to ∼80% of melting temperature. Significant dissipation (0.077 ≤ Q−1(ω) ≤ 0.488) is observed along with frequency dependent softening of zinc's Young's modulus and an extremely small activation energy for creep (⩽7 kJ mol−1). In addition, during sinusoidal deformation the original microstructure is replaced by one with a reduced dislocation density and small, uniform, grain size. This combination of behavior collectively reflects a mode of deformation called “internal stress superplasticity”; this deformation mechanism is unique to anisotropic materials and activated by cyclic loading generating large internal stresses. Here we observe a new form of internal stress superplasticity, which we name as “elastic strain mismatch superplasticity.” In it the large stresses are caused by the compressional anisotropy. If this mechanism is also active in hcp-iron and the Earth's inner-core it will be a contributor to inner-core observed seismic attenuation and constrain the maximum inner-core grain-size to ≲10 km.
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Jun 2024
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B18-Core EXAFS
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Diamond Proposal Number(s):
[20379, 22735, 24947]
Open Access
Abstract: In this paper, we address two key features of the behaviour of Fe-rich amphibole at high temperatures: (1) the Fe2+ → Fe3+ + e− exchange within the crystal bulk, and (2) the consequent rise in electrical conductivity. Cycling heating-cooling experiments were done in situ up to 542 °C (815 K) at beamline B11 of the Diamond Synchrotron Laboratory (UK). X-ray absorption spectra at the Fe K-edge and electrical resistivity were measured simultaneously on a single crystal of riebeckite with a composition very close to the ideal formula A□BNa2C(Fe2+3Fe3+2)TSi8O22W(OH)2. The Fe3+/Fetot ratio was monitored via analysis of the pre-edge feature in the XANES spectra. Our data show slight oscillations of the oxidation state of Fe with temperature cycling up to around 400 °C (673 K), followed by a substantial gradual increase in Fe2+ → Fe3+ oxidation that starts at ~450 °C (~723 K) and is completed at ~525 °C (~798 K). The conductivity (σ) measured along the crystallographic c-axis oscillates strongly with cycling temperature allowing us to conclude that it is intrinsically related to the electron hopping induced by thermal treatment. The activation-energy derived from the σ(T) trend is Ea = 74.4 ± 0.6 kJ/mol (0.77 ± 0.01 eV), in agreement with small-polaron conduction. This study provides direct and robust support of the conduction mechanisms in Fe-amphibole previously inferred from indirect methods. Given that riebeckite is a significant component in the glaucophanitic amphiboles common in blueschists associated with subducted oceanic crust, our data provide a link between atomic-scale processes and Earth-scale anomalous conductivity observed via geophysical measurements.
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Oct 2023
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I12-JEEP: Joint Engineering, Environmental and Processing
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Abstract: In this study, we present experimental investigations on a low-porosity bioclastic calcarenite from the Cotiella Basin in the Spanish Pyrenees. Our objective is to elucidate the dominant failure mechanisms during the laboratory reactivation of natural deformation bands oriented at various angles to the maximum principal stress (σ1) direction. Triaxial compression experiments were conducted at the I12-JEEP beamline of the Diamond Light Source, UK, using a modified version of the Mjolnir cell employed by Cartwright-Taylor et al. (2022). Moreover, 4D (space and time-resolved) X-ray computed tomography images were acquired at 8 μm3 voxel size resolution during the triaxial compression tests (10 MPa to 30 MPa confining pressure).
Our mechanical data show that the presence of natural deformation features within the tested samples influences the material's strength. When comparing intact samples of the host rock under the same confining pressures, we observed that these samples exhibit higher peak stresses as opposed to those containing natural deformation features. Our research reveals that new deformation bands are formed as the angle (θ) between the deformation bands and σ1 increases. In this low-porosity carbonate, the reactivation of pre-existing deformation bands only occurs when their dipping angles are close to 70o.
To investigate the spatial and temporal relationships among naturally occurring and laboratory induced deformation bands and fractures, we employed time-resolved X-ray CT and Digital Volume Correlation (Figure 1). Utilizing the SPAM open-source software (Stamati et al., 2020), we calculated the volumetric and shear strain fields. The orientation of the laboratory-induced failure planes is influenced by the orientation, width, and presence (or absence) of porosity along the length of the pre-existing natural bands. Additionally, the pre-existing secondary deformation features may contribute to additional mechanical damage, which can either facilitate the development or divert the newly formed failure planes.
In summary, our findings emphasize that the presence of natural deformation features weakens the material. We also observe that the reactivation of pre-existing bands occurs primarily at dipping angles near 70o in this low-porosity carbonate. The use of advanced imaging techniques and the SPAM software have allowed us to explore the relationships between the naturally occurring and laboratory-induced deformation features, highlighting the influence of orientation, width, and porosity on the orientation of failure planes. Finally, the presence of pre-existing deformation features triggers additional mechanical damage, affecting the development and direction of new failure planes.
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Oct 2023
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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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