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With the goal of better understanding stimulation in crystalline rock for improving enhanced geothermal systems (EGS), the EGS Collab Project performed a series of stimulations and flow tests at 1.25 and 1.5 km depths. The tests were performed in two well-instrumented testbeds in the Sanford Underground Research Facility in Lead, South Dakota, United States. The testbed for Experiment 1 at 1.5 km depth contained two open wells for injection and production and six instrumented monitoring wells surrounding the targeted stimulation zone. Four multi-step stimulation tests targeting hydraulic fracturing and nearly year-long ambient temperature and chilled water flow tests were performed in Experiment 1. The testbed for Experiments 2 and 3 was at 1.25 km depth and contained five open wells in an outwardly fanning five-spot pattern and two fans of well-instrumented monitoring wells surrounding the targeted stimulation zone. Experiment 2 targeted shear stimulation, and Experiment 3 targeted low-flow, high-flow, and oscillating pressure stimulation strategies. Hydraulic fracturing was successful in Experiments 1 and 3 in generating a connected system wherein injected water could be collected. However, the resulting flow was distributed dynamically, and not entirely collected at the anticipated production well. Thermal breakthrough was not observed in the production well, but that could have been masked by the Joule-Thomson effect. Shear stimulation in Experiment 2 did not occur – despite attempting to pressurize the fractures most likely to shear – because of the inability to inject water into a mostly-healed fracture, and the low shear-to-normal stress ratio. The EGS Collab experiments are described to provide a background for lessons learned on topics including induced seismicity, the correlation between seismicity and permeability, distributed and dynamic flow systems, thermoelastic and pressure effects, shear stimulation, local geology, thermal breakthrough, monitoring stimulation, grouting boreholes, modeling, and system management.

Undocumented Orphaned Wells (UOWs) are wells without an operator that have limited or no documentation with regulatory authorities. An estimated 310,000 to 800,000 UOWs exist in the United States (US), whose locations are largely unknown. These wells can potentially leak methane and other volatile organic compounds to the atmosphere, and contaminate groundwater. In this study, we developed a novel framework utilizing a state-of-the-art computer vision neural network model to identify the precise locations of potential UOWs. The U-Net model is trained to detect oil and gas well symbols in georeferenced historical topographic maps, and potential UOWs are identified as symbols that are further than 100 m from any documented well. A custom tool was developed to rapidly validate the potential UOW locations. We applied this framework to four counties in California and Oklahoma, leading to the discovery of 1301 potential UOWs across >40,000 km2. We confirmed the presence of 29 UOWs from satellite images and 15 UOWs from magnetic surveys in the field with a spatial accuracy on the order of 10 m. This framework can be scaled to identify potential UOWs across the US since the historical maps are available for the entire nation.

The EGS Collab project acquired continuous active-source seismic monitoring (CASSM) data before, during, and after hydraulic stimulations at the first testbed at the depth of 4850 ft (1478 m) at the Sanford Underground Research Facility in Lead, South Dakota, for monitoring fracture creation and evolution. CASSM acquisition was conducted using 24 hydrophones, 18 accelerometers, and 17 piezoelectric sources within four fracture-parallel wells and two orthogonal wells. 3D anisotropic traveltime tomography and anisotropic elastic-waveform inversion of the campaign cross-borehole seismic data show that the rock within the stimulation region is a heterogeneous horizontal transverse isotropic medium. We use these inversion results as the initial models and apply 3D anisotropic first-arrival traveltime tomography and 3D anisotropic elastic-waveform inversion to the CASSM data acquired after each stimulation in May, 2018 and December, 2018. We observe the spatiotemporal evolution of seismic velocities and anisotropic parameters caused by hydraulic fracture stimulations, showing the regions of rock alternation caused by hydraulic fracture stimulation.

Fracture injection/shut-in tests are commonly used to measure the state of stress in the subsurface. Injection creates a hydraulic fracture (or in some cases, opens a preexisting fracture), and then the pressure after shut-in is monitored to identify fracture closure. Different interpretation procedures have been proposed for estimating closure, and the procedures sometimes yield significantly different results. In this study, direct, in-situ strain measurements are used to observe fracture reopening and closure. The tests were performed as part of the EGS Collab project, a mesoscale project performed at 1.25 and 1.5 km depth at the Sanford Underground Research Facility. The tests were instrumented with the SIMFIP tool, a double-packer probe with a high-resolution three-dimensional borehole displacement sensor. The measurements provide a direct observation of the fracture closure signature, enabling a high-fidelity estimate of the fracture closure stress (ie, the normal stress on the fracture). In two of the four tests, injection created an opening mode fracture, and so the closure stress can be interpreted as the minimum principal stress. In the other two tests, injection probably opened preexisting natural fractures, and so the closure stress can be interpreted as the normal stress on the fractures. The strain measurements are compared against different proposed methods for estimating closure stress from pressure transients. The shut-in transients are analyzed with two techniques that are widely used in the field of petroleum engineering – the ‘tangent’ method and the ‘compliance’ method. In three of the four tests, the tangent method significantly underestimates the closure stress. The compliance method is reasonably accurate in all four tests. Closure stress is also interpreted using two other commonly-used methods – ‘first deviation from linearity’ and the method of (Hayashi and Haimson, 1991). In comparison with the SIMFIP data, these methods tend to overestimate the closure stress, evidently because they identify closure from early-time transient effects, such as near-wellbore tortuosity. In two of the tests, microseismic imaging provides an independent estimate of the size of the fracture created by injection. When combined with a simple mass balance calculation, the SIMFIP stress measurements yield predictions of fracture size that are reasonably consistent with the estimates from microseismic. The calculations imply an apparent fracture toughness 2-3x higher than typical laboratory-derived values.

Fundamental mechanical and creep behavior of minerals at elevated temperatures is relevant to many subsurface exploration and resource recovery processes, yet remains largely elusive. This study uses instrumented indentation to measure microscale deformation and nanoscale creep of biotite, albite, and quartz, which are the major mineral phases of granitic rocks, at temperatures up to 400 °C. The results show that the elastic modulus of biotite is not only the lowest at room temperature but also decays the most at elevated temperature (i.e., by 25% reduction at 400 °C) compared to that of albite and quartz. The creep deformation within 20 s doubles when the temperature increases from 20 °C to 400 °C for albite, quartz, and biotite, and biotite showed at least three times the overall creep deformation compared to quartz and albite under the same temperature. The indentation creep deformation can be well characterized using a logarithmic time model, showing both transient and constant-rate creep deformation. The secondary creep rate for biotite is about three times that of albite and quartz at the same temperature, and as the temperature increases from 20 °C to 400 °C, the rate of secondary creep becomes approximately 10 times faster for the three tested minerals. Both transient creep deformation and the rate of secondary creep can be empirically correlated to the elastic moduli, which allows quick estimates of the temperature-dependent creep behavior of granitic minerals using their elastic properties, especially when those creep constants are not readily available at elevated temperatures. These results enhance the understanding of temperature-dependent creep deformation at small scales and provide insight into mineral-level damage in granitic rocks due to temperature and long-term deformation.

The behavior of heated bentonite buffer is critical for the security and long-term performance of a geological repository for high-level radioactive waste (HLW). While laboratory column experiments have been conducted to investigate compacted bentonite and coupled THMC (thermal-hydro-mechanical and chemical) processes for a moderate temperature range of up to 100 °C, data for a higher temperature range are limited. Understanding bentonite behavior and coupled THMC processes under higher temperatures (e.g., up to 200 °C) could allow for a more economic repository design and would expand the data and knowledge base for more reliable modeling. In this study, a bench-scale experiment was conducted in a compacted bentonite column experiencing both heating up to 200 °C in the center and hydration from a sand-clay boundary surrounding the column. During the experiment run for 1.5 years, frequent X-ray computed tomography (CT) scanning of bentonite provided insights into the spatiotemporal evolution of (1) hydration/dehydration, (2) clay swelling/shrinkage, (3) displacement, and (4) mineral precipitation. After the experiment, a comprehensive post-dismantling characterization of bentonite samples was conducted. Results showed that the bentonite hydration was axi-symmetrical despite the initial heterogeneity due to packing, confirming the ability of bentonite to seal fast flow/transport paths. Compared to a non-heated control experiment, the heated column showed greater CT density variations along the radial distance, indicating that homogenization of bentonite might be more difficult if a temperature gradient is maintained in the repository. Precipitation of an anhydrite layer occurred in the inner hot zone, pointing to potential concerns about salt precipitation causing canister corrosion. Ultimately, the experiments provided a high-resolution window into the strongly dynamic and coupled behavior of bentonite exposed to heating, hydration and swelling, which will be valuable for improving modeling of coupled processes, especially for the early state of a HLW repository.

The water-gas relative permeability is an important parameter to characterize multiphase flow in sediments. To study the water-gas relative permeability of hydrate-bearing porous media, multiphase flow simulations were carried out at the pore scale using the lattice Boltzmann method. The effects of hydrate saturation and hydrate-growth habits on the water-gas relative permeability, which is scaled by the relative permeability considering the hydrate only, were evaluated in a two-dimensional porous medium. Results show that the increase of hydrate saturation causes the decrease of water-gas effective permeability as expected. However, the effect of hydrate saturation on the water-gas relative permeability is different from that of hydrate saturation on the water-gas effective permeability. The water-gas relative permeability increases with the increase of hydrate saturation in the pore-filling case. The water-gas relative permeability decreases with the increase of hydrate saturation in the grain-coating case. The wettability of solid phase has a different effect on the relative permeability of wetting phase and nonwetting phase. The Jamin effect (phase blocking) was observed and may exist in the production of gas from natural gas hydrate reservoirs. This seriously affects the multiphase flow characteristics. The changes of microscale fluid distribution effect the changes of water-gas relative permeability. The relationship between the water-gas relative permeability and the characterization parameters of microscale fluid distribution was analyzed.

Enhanced geothermal systems (EGS) offer the potential for a much larger energy source than conventional hydrothermal systems. Hot, low-permeability rocks are prevalent at depth around the world, but the challenge of extracting thermal energy depends on the ability to create and sustain open fracture networks. Laboratory experiments were conducted using a suite of selected rock cores (granite, metasediment, rhyolite ash-flow tuff, and silicified rhyolitic tuff) at relevant pressures (uniaxial loading up to 20.7 MPa and fluid pressures up to 10.3 MPa) and temperatures (150-250 °C) to evaluate the potential impacts of circulating fluids through fractured rock by monitoring changes in fracture aperture, mineralogy, permeability, and fluid chemistry. Because a fluid in disequilibrium with the rocks (deionized water) was used for these experiments, there was net dissolution of the rock sample: This increased with increasing temperature and experiment duration. Thermal-hydrological-mechanical-chemical (THMC) modeling simulations were performed for the rhyolite ash-flow tuff experiment to test the ability to predict the observed changes. These simulations were performed in two steps: A thermal-hydrological-mechanical (THM) simulation to evaluate the effects of compression of the fracture, and a thermal-hydrological-chemical (THC) simulation to evaluate the effects of hydrothermal reactions on the fracture mineralogy, porosity, and permeability. These experiments and simulations point out how differences in rock mineralogy, fluid chemistry, and geomechanical properties influence how long asperity-propped fracture apertures may be sustained. Such core-scale experiments and simulations can be used to predict EGS reservoir behavior on the field scale.

In cryogenic fracturing, a rock surface exposed to cryogenic fluids undergoes a large thermal gradient, and the resultant local tensile stress overcomes rock strength and initiates fractures. This study investigates the development of cracks generated from the cryogenic treatment of a borehole under no external confining stress on specimens. The experiments were performed on transparent PMMA specimens to observe fracture proliferation around boreholes. Liquid nitrogen was flowed through the boreholes to cool the borehole surface. The results show that initial fracture growth is characterized by abrupt starts and stops, and as the fracture propagates outward, the growth appears more continuous. In an early stage, horizontal/radial fractures and vertical fractures are the defining patterns. Horizontal fractures tend to be separated by a specific exclusion distance (i.e., spacing between cracks). While distinct horizontal/vertical fractures and exclusion distance manifest themselves at an early stage, fractures resulting from fracture interactions and curvatures can develop into complex shapes at later stages. Cryogenic thermal loading induces distinctively curved fractures. The tendency of curvature may prevent greater penetration. An increase in the borehole pressure during liquid nitrogen flow, however, can lessen fracture tortu-osity and facilitate radial propagation. A high flow pressure and rate are also advantageous in that they accelerate cooling and fracture propagation.

Oil and gas shales are a system where understanding the mechanical properties at the microscale is of paramount importance, e.g. to better understand the behavior of proppant-shale contacts and their role in the evolution of propped fractures in unconventional reservoirs. This work shows for the first time an experiment coupling indentation testing with in situ X-ray imaging in a Green River shale sample. A full compliance curve has been measured with the sample in water, allowing to visualize the indentation of the sample in function of axial load, in a purpose-built system for combined in situ indentation and X-ray imaging. A series of 3D datasets were used for a digital volume correlation study to obtain local strain fields. This analysis has been complemented with the analysis of cracks. Finally, geomechanical modeling has been carried out to replicate and generalize the observed behavior in the shale. This study validated this experimental approach, providing a breakthrough in understanding micro-mechanics in shales, and demonstrates how this class of experiments can be important for studies involving the prediction of the evolution of propped fractures in shale reservoirs, with possible applications in a much larger number of application fields (geothermal, materials science, etc.)

Estimation of CO2 storage capacity in fractured porous reservoirs requires a better understanding of the CO2-water flow fundamentals in fracture-matrix systems. There are few core-flood experiments on three-dimensional CO2-water drainage in a fracture-matrix system, yet none have examined the impacts of the capillary continuity of fractures and fracture-matrix interactions. In this study, twelve drainage experiments were conducted in four fracture-matrix columns, each comprising a vertical stack of a cylindrical rock core, a filter paper serving as an analogue to a horizontal fracture, and a ceramic plate. The core sample was surrounded by open space at the top and circumferential sides to model fractures, allowing for 3-D CO2-water drainage in the rock core and displaced water draining across the horizontal fracture. X-ray computed tomography was conducted to visualize the dynamic invasion/drainage processes in four rock core samples showing contrasts in anisotropy, permeability, and heterogeneity. Experimental results show (1) the equilibrium CO2 saturations in the rock matrix vary from 0.10 to 0.60 at controlled capillary pressures up to 200 kPa, (2) the CO2 saturations in the matrix increaze with water saturation in the horizontal fracture resulting in better capillary continuity for water to drain across the fracture, and (3) the fracture water saturation can be enhanced by the non-uniform fracture capillary pressure and countercurrent flow of CO2 and water across the fracture-matrix interface. In the case of high fracture water saturation, matrix CO2 saturation largely depends on matrix anisotropy and heterogeneity. The core-scale experimental results contribute to understand the fracture-matrix interactions and CO2 storage efficiency in fractured porous media.

This paper describes a new modeling framework for microscopic to reservoir-scale simulations of hydraulic fracturing and production. The approach builds upon a fusion of two existing high-performance simulators for reservoir-scale behavior: the GEOS code for hydromechanical evolution during stimulation and the TOUGH+ code for multi-phase flow during production. The reservoir-scale simulations are informed by experimental and modeling studies at the laboratory scale to incorporate important micro-scale mechanical processes and chemical reactions occurring within the fractures, the shale matrix, and at the fracture-fluid interfaces. These processes include, among others, changes in stimulated fracture permeability as a result of proppant behavior rear-rangement or embedment, or mineral scale precipitation within pores and microfractures, at µm to cm scales. In our new modeling framework, such micro-scale testing and modeling provides upscaled hydromechanical parameters for the reservoir scale models. We are currently testing the new modeling framework using field data and core samples from the Hydraulic Fracturing Field Test (HFTS), a recent field-based joint research experiment with intense monitoring of hydraulic fracturing and shale production in the Wolfcamp Formation in the Permian Basin (USA). Below, we present our approach coupling the reservoir simulators GEOS and TOUGH+ informed by upscaled parameters from micro-scale experiments and modeling. We provide a brief overview of the HFTS and the available field data, and then discuss the ongoing application of our new workflow to the HFTS data set.

In cryogenic fracturing, a rock surface exposed to cryogenic fluids undergoes a large thermal gradient, and the resultant local tensile stress overcomes rock strength and initiates fractures. This study investigates the development of cracks generated from the cryogenic treatment of a borehole under no external confining stress on specimens. The experiments were performed on transparent PMMA specimens to observe fracture proliferation around boreholes. Liquid nitrogen was flowed through the boreholes to cool the borehole surface. The results show that initial fracture growth is characterized by abrupt starts and stops, and as the fracture propagates outward, the growth appears more continuous. In an early stage, horizontal/radial fractures and vertical fractures are the defining patterns. Horizontal fractures tend to be separated by a specific exclusion distance (i.e., spacing between cracks). While distinct horizontal/vertical fractures and exclusion distance manifest themselves at an early stage, fractures resulting from fracture interactions and curvatures can develop into complex shapes at later stages. Cryogenic thermal loading induces distinctively curved fractures. The tendency of curvature may prevent greater penetration. An increase in the borehole pressure during liquid nitrogen flow, however, can lessen fracture tortu-osity and facilitate radial propagation. A high flow pressure and rate are also advantageous in that they accelerate cooling and fracture propagation.

This paper describes a new modeling framework for microscopic to reservoir-scale simulations of hydraulic fracturing and production. The approach builds upon a fusion of two existing high-performance simulators for reservoir-scale behavior: the GEOS code for hydromechanical evolution during stimulation and the TOUGH+ code for multi-phase flow during production. The reservoir-scale simulations are informed by experimental and modeling studies at the laboratory scale to incorporate important micro-scale mechanical processes and chemical reactions occurring within the fractures, the shale matrix, and at the fracture-fluid interfaces. These processes include, among others, changes in stimulated fracture permeability as a result of proppant behavior rear-rangement or embedment, or mineral scale precipitation within pores and microfractures, at µm to cm scales. In our new modeling framework, such micro-scale testing and modeling provides upscaled hydromechanical parameters for the reservoir scale models. We are currently testing the new modeling framework using field data and core samples from the Hydraulic Fracturing Field Test (HFTS), a recent field-based joint research experiment with intense monitoring of hydraulic fracturing and shale production in the Wolfcamp Formation in the Permian Basin (USA). Below, we present our approach coupling the reservoir simulators GEOS and TOUGH+ informed by upscaled parameters from micro-scale experiments and modeling. We provide a brief overview of the HFTS and the available field data, and then discuss the ongoing application of our new workflow to the HFTS data set.

There is an interest to ensure sub-saturated water content in lines containing carbon dioxide in applications such as enhanced oil recovery and carbon sequestration, to reduce risks of hydrate blockage and corrosion. The water content of carbon dioxide at various temperatures and pressures has been measured in the past, but there is no consistent set of measurements that could be used for carbon dioxide storage and transportation design work. The solubility of water in a carbon dioxide rich gas phase at hydrate forming conditions was measured in this work. Pressures ranged from 12.06 to 29.30 bar along two isotherms, 1 °C and −7 °C, all within the gaseous carbon dioxide and hydrate stability zone. For the first time in these types of measurements, the solid phase was also characterized and confirmed to be carbon dioxide hydrate via X-ray computed tomography, simultaneous with water content measurements of the gas phase. Once carbon dioxide hydrate conversion had reached a maximum value (65% estimated by X-ray computed tomography), the equilibrium water content was measured. Prior to reaching this maximum carbon dioxide hydrate conversion, the water content in carbon dioxide was observed to decrease as liquid water converted to carbon dioxide hydrate. This slow conversion to hydrate, metastability of the hydrate phase, or unexpected phases may be responsible for the large discrepancy between prior data sets for similar carbon dioxide water content measurements.

Reliable estimations of the relative permeability of gas and water in hydrate-bearing sediments (HBS) and the dependency of the relative permeability on hydrate saturation are critical to predict the productivity of a hydrate reservoir. Yet, this remains poorly estimated owing to lack of experimental data associated with difficulties in conducting multiphase flow experiments in HBS. Recognizing the experimental challenges, this study intends to develop and validate a new experimental system and procedure of unsteady-state relative permeability test that can generate reliable and reproducible flow measurements in HBS. Gas hydrate is considered as a part of solid matrix in the sediment, so one of the challenges is to maintain a constant hydrate saturation, which is achieved in this experimental study using tight pressure-temperature (P-T) control near the hydrate stability boundary. The measured differential pressure across the specimen, methane injection flow rate, and volume of displaced brine are used to calculate the relative permeability by adopting a conventional Buckley-Leverett theory-based interpretation method. Residual brine saturation calculated for the hydrate-bearing specimen is higher than that of hydrate-free specimen, presumably due to decrease in pore size, increase in heterogeneity of solid matrix, and increase in size distribution of solid matrix and pore in the presence of hydrates. Further studies are necessary to represent the results of the unsteady-state flow experiment in HBS with a gas hydrate-dependent relative permeability model.

Reliable estimations of the relative permeability of gas and water in hydrate-bearing sediments (HBS) and the dependency of the relative permeability on hydrate saturation are critical to predict the productivity of a hydrate reservoir. Yet, this remains poorly estimated owing to lack of experimental data associated with difficulties in conducting multiphase flow experiments in HBS. Recognizing the experimental challenges, this study intends to develop and validate a new experimental system and procedure of unsteady-state relative permeability test that can generate reliable and reproducible flow measurements in HBS. Gas hydrate is considered as a part of solid matrix in the sediment, so one of the challenges is to maintain a constant hydrate saturation, which is achieved in this experimental study using tight pressure-temperature (P-T) control near the hydrate stability boundary. The measured differential pressure across the specimen, methane injection flow rate, and volume of displaced brine are used to calculate the relative permeability by adopting a conventional Buckley-Leverett theory-based interpretation method. Residual brine saturation calculated for the hydrate-bearing specimen is higher than that of hydrate-free specimen, presumably due to decrease in pore size, increase in heterogeneity of solid matrix, and increase in size distribution of solid matrix and pore in the presence of hydrates. Further studies are necessary to represent the results of the unsteady-state flow experiment in HBS with a gas hydrate-dependent relative permeability model.

Geological carbon storage in deep aquifers involves displacement of resident brine by supercritical CO2 (scCO2), which is an unstable drainage process caused by the invasion of less viscous scCO2. The unstable drainage is greatly complicated by aquifer heterogeneity and anisotropy and regarded as one of the key factors accounting for the uncertainty in storage capacity estimates. The impacts of pore-scale characteristics on the unstable drainage remain poorly understood. In this study, scCO2 drainage experiments were conducted at 40 °C and 9 MPa using a homogeneous elliptical micromodel with low or high anisotropy, a homogeneous/isotropic hexagonal micromodel, and a heterogeneous sandstone-analog micromodel. Each initially water-saturated micromodel was invaded by scCO2 at different rates with logCa (the capillary number)ranging from −7.6 to −4.4, and scCO2/water images were obtained. The measured CO2 saturations in these centimeter-scale micromodels vary considerably from 0.08 to 0.93 depending on the pore-scale characteristics and capillary number. It was also observed that scCO2 drainage follows the classic flow-regime transition from capillary fingering through crossover to viscous fingering for either of the low-anisotropy elliptical and heterogeneous micromodels, but with disparate crossover zones. The crossover zones of scCO2 saturation were then unified with the minimum scCO2 saturation occurring at logCa*=-4.0 using the complete capillary number (Ca*)that considers pore characteristics. For the hexagonal and the high-anisotropy elliptical micromodels, a monotonic increase in scCO2 saturation with increasing Ca* (without crossover)was observed. It appears that the complete capillary number is more appropriate than the classic capillary number when characterizing flow regimes and CO2 saturation in different pore networks.

Geological carbon storage in deep aquifers involves displacement of resident brine by supercritical CO2 (scCO2), which is an unstable drainage process caused by the invasion of less viscous scCO2. The unstable drainage is greatly complicated by aquifer heterogeneity and anisotropy and regarded as one of the key factors accounting for the uncertainty in storage capacity estimates. The impacts of pore-scale characteristics on the unstable drainage remain poorly understood. In this study, scCO2 drainage experiments were conducted at 40 °C and 9 MPa using a homogeneous elliptical micromodel with low or high anisotropy, a homogeneous/isotropic hexagonal micromodel, and a heterogeneous sandstone-analog micromodel. Each initially water-saturated micromodel was invaded by scCO2 at different rates with logCa (the capillary number)ranging from −7.6 to −4.4, and scCO2/water images were obtained. The measured CO2 saturations in these centimeter-scale micromodels vary considerably from 0.08 to 0.93 depending on the pore-scale characteristics and capillary number. It was also observed that scCO2 drainage follows the classic flow-regime transition from capillary fingering through crossover to viscous fingering for either of the low-anisotropy elliptical and heterogeneous micromodels, but with disparate crossover zones. The crossover zones of scCO2 saturation were then unified with the minimum scCO2 saturation occurring at logCa*=-4.0 using the complete capillary number (Ca*)that considers pore characteristics. For the hexagonal and the high-anisotropy elliptical micromodels, a monotonic increase in scCO2 saturation with increasing Ca* (without crossover)was observed. It appears that the complete capillary number is more appropriate than the classic capillary number when characterizing flow regimes and CO2 saturation in different pore networks.

The organic and mineralogical heterogeneity in shale at micrometer and nanometer spatial scales contributes to the quality of gas reserves, gas flow mechanisms and gas production. Here, we demonstrate two molecular imaging approaches based on infrared spectroscopy to obtain mineral and kerogen information at these mesoscale spatial resolutions in large-sized shale rock samples. The first method is a modified microscopic attenuated total reflectance measurement that utilizes a large germanium hemisphere combined with a focal plane array detector to rapidly capture chemical images of shale rock surfaces spanning hundreds of micrometers with micrometer spatial resolution. The second method, synchrotron infrared nano-spectroscopy, utilizes a metallic atomic force microscope tip to obtain chemical images of micrometer dimensions but with nanometer spatial resolution. This chemically "deconvoluted" imaging at the nano-pore scale is then used to build a machine learning model to generate a molecular distribution map across scales with a spatial span of 1000 times, which enables high-throughput geochemical characterization in greater details across the nano-pore and micro-grain scales and allows us to identify co-localization of mineral phases with chemically distinct organics and even with gas phase sorbents. This characterization is fundamental to understand mineral and organic compositions affecting the behavior of shales.

The performance of geologic CO2 sequestration (GCS) can be affected by CO2 mineralization and changes in the permeability of geologic formations resulting from interactions between water-bearing supercritical CO2 (scCO2) and silicates in reservoir rocks. However, without an understanding of the size effects, the findings in previous studies using nanometer- or micrometer-size particles cannot be applied to the bulk rock in field sites. In this study, we report the effects of particle sizes on the carbonation of wollastonite (CaSiO3) at 60 °C and 100 bar in water-bearing scCO2. After normalization by the surface area, the thickness of the reacted wollastonite layer on the surfaces was independent of particle sizes. After 20 h, the reaction was not controlled by the kinetics of surface reactions but by the diffusion of water-bearing scCO2 across the product layer on wollastonite surfaces. Among the products of reaction, amorphous silica, rather than calcite, covered the wollastonite surface and acted as a diffusion barrier to water-bearing scCO2. The product layer was not highly porous, with a specific surface area 10 times smaller than that of the altered amorphous silica formed at the wollastonite surface in aqueous solution. These findings can help us evaluate the impacts of mineral carbonation in water-bearing scCO2.

Niobrara shale cubes of 20 cm from Colorado were employed to investigate gas and supercritical CO2 injection-induced fracturing in naturally fractured caprocks of deep aquifers/depleted reservoirs and fractured shale reservoirs. Under tri-axial stresses, gas or supercritical CO2 was injected into the center of the cubes to induce fracturing. Real-time pressure and temperature, acoustic wave, pressure decay, fracture coloring, and gas fracturing were used to characterize the fracturing process and fracture morphology. Without pore pressure, CO2 injection-induced fracturing occurred and completed instantly, accompanied by an evident temperature drop. Strongly bonded fractures barely affected transverse fracture propagation, whereas weakly bonded or open fractures arrested the injected fluid first and then allowed it to generate new fractures perpendicular to the minimum horizontal stress. Breakdown pressures for cubes with preexisting fractures using gas and supercritical CO2 are much lower than both poroelastic predictions and slick-water fracturing pressure, and some are even lower than the minimum horizontal stress. This is attributed to unconformable preexisting fractures and the low viscosity of CO2. Moreover, decreasing tri-axial stress levels and increasing stress differences tend to lower the breakdown pressure. This study is instructive for understanding and tackling geomechanical issues related to CO2 geological storage and fracturing of shale reservoirs.

Leakage risk assessment is an inevitable procedure in permanent sequestration and storage of CO2 in deep saline aquifers and depleted oil and gas reservoirs, where the integrity of caprock is most critical. Low porosity and low permeability concrete cubes were employed as caprock analogs to investigate the supercritical CO2 injection-induced fracturing processes under true tri-axial stress conditions. A systematic experimental procedure, consisting of active acoustic emission measurement, pressure decay, injection pressure and temperature monitoring, fracture coloring, and gas fracturing, is formulated to qualitatively and quantitatively characterize the injection-induced fracturing processes and fracture morphology. Occurrence of injection-induced fracturing can be directly identified from peaks of borehole pressure profiles as well as sharp drops on temperature profiles due to CO2 expansion, but generally there was no fracture propagation plateau appearing for the 20 cm rock cubes with zero pore pressure. Acoustic wave signatures, including both waveform change and arrival time delay, can effectively capture the extension of induced fractures inside the opaque rock. Initiation and propagation of supercritical CO2 injection-induced fractures are highly dominated by the tri-axial stresses, following the general trend of continuum mechanics at high stress levels with large stress difference. As the stress difference decreases, induced fractures branch off in relatively arbitrary directions. For these supercritical CO2 injection-induced fracturing experiments, poroelastic mechanics model makes a decent fit with the measured breakdown pressure of the caprock analogs. Findings in this study are valuable for risk analysis and operation optimization of geological CO2 sequestration and storage as well as for CO2 fracturing design and implementation in shale and tight reservoirs.

The concept of cryogenic fracturing is that a sharp thermal gradient developed by applying a cryogenic fluid on a rock surface causes a strong local tensile stress that initiates fractures. Prior field tests suggest that field application with special equipment rated for cryogenic temperatures may deliver potential benefits. The tests did not, however, identify the fracture mechanisms at work in downhole conditions. In this study, we present our laboratory designs and procedures developed for studying cryogenic fracturing mechanisms in a well environment, and examine typical data indicative of the performance of the system. The experimental apparatus and procedures were specifically designed to conduct cryogenic fracturing tests in specimens under confining stress, with integrated cryogen transport, measurements, and fracture characterization. A true-triaxial loading system was built to simulate reservoir stress levels and anisotropic stress application, and was designed to avoid thermal stresses in tests involving cryogen by arranging discrete components in an open chamber. To maximize thermal shock on the wellbore surface, tubing and wellhead are configured so that liquid nitrogen enters the borehole and flow out after contributing to thermal shock. The temperature at boreholes and along flow lines, borehole pressure, and liquid nitrogen consumption are monitored throughout treatments. Acoustic transmission and pressure-decay measurements are used to characterize fractures before and after the experiments. Breakdown tests performed on un-stimulated specimens and stimulated specimens compare breakdown pressures of the two groups and thus evaluate the performance of thermal fracturing. The laboratory design was able to effectively apply cryogenic stimulations to laboratory rock specimens. The characterization methods were able to capture fracture creation and rock property changes due to cryogenic fracturing.

Leakage risk assessment is an inevitable procedure in permanent sequestration and storage of CO2 in deep saline aquifers and depleted oil and gas reservoirs, where the integrity of caprock is most critical. Low porosity and low permeability concrete cubes were employed as caprock analogs to investigate the supercritical CO2 injection-induced fracturing processes under true tri-axial stress conditions. A systematic experimental procedure, consisting of active acoustic emission measurement, pressure decay, injection pressure and temperature monitoring, fracture coloring, and gas fracturing, is formulated to qualitatively and quantitatively characterize the injection-induced fracturing processes and fracture morphology. Occurrence of injection-induced fracturing can be directly identified from peaks of borehole pressure profiles as well as sharp drops on temperature profiles due to CO2 expansion, but generally there was no fracture propagation plateau appearing for the 20 cm rock cubes with zero pore pressure. Acoustic wave signatures, including both waveform change and arrival time delay, can effectively capture the extension of induced fractures inside the opaque rock. Initiation and propagation of supercritical CO2 injection-induced fractures are highly dominated by the tri-axial stresses, following the general trend of continuum mechanics at high stress levels with large stress difference. As the stress difference decreases, induced fractures branch off in relatively arbitrary directions. For these supercritical CO2 injection-induced fracturing experiments, poroelastic mechanics model makes a decent fit with the measured breakdown pressure of the caprock analogs. Findings in this study are valuable for risk analysis and operation optimization of geological CO2 sequestration and storage as well as for CO2 fracturing design and implementation in shale and tight reservoirs.

During the past two decades, hydraulic fracturing has significantly improved oil and gas production from shale and tight sandstone reservoirs in the United States and elsewhere. Considering formation damage, water consumption, and environmental impacts associated with water-based fracturing fluids, efforts have been devoted to developing waterless fracturing technologies because of their potential to alleviate these issues. Herein, key theories and features of waterless fracturing technologies, including Oil-based and CO2 energized oil fracturing, explosive and propellant fracturing, gelled LPG and alcohol fracturing, gas fracturing, CO2 fracturing, and cryogenic fracturing, are reviewed. We then experimentally elaborate on the efficacy of liquid nitrogen in enhancing fracture initiation and propagation in concrete samples, and shale and sandstone reservoir rocks. In our laboratory study, cryogenic fractures generated were qualitatively and quantitatively characterized by pressure decay tests, acoustic measurements, gas fracturing, and CT scans. The capacity and applicability of cryogenic fracturing using liquid nitrogen are demonstrated and examined. By properly formulating the technical procedures for field implementation, cryogenic fracturing using liquid nitrogen could be an advantageous option for fracturing unconventional reservoirs.

During the past two decades, hydraulic fracturing has significantly improved oil and gas production from shale and tight sandstone reservoirs in the United States and elsewhere. Considering formation damage, water consumption, and environmental impacts associated with water-based fracturing fluids, efforts have been devoted to developing waterless fracturing technologies because of their potential to alleviate these issues. Herein, key theories and features of waterless fracturing technologies, including Oil-based and CO2 energized oil fracturing, explosive and propellant fracturing, gelled LPG and alcohol fracturing, gas fracturing, CO2 fracturing, and cryogenic fracturing, are reviewed. We then experimentally elaborate on the efficacy of liquid nitrogen in enhancing fracture initiation and propagation in concrete samples, and shale and sandstone reservoir rocks. In our laboratory study, cryogenic fractures generated were qualitatively and quantitatively characterized by pressure decay tests, acoustic measurements, gas fracturing, and CT scans. The capacity and applicability of cryogenic fracturing using liquid nitrogen are demonstrated and examined. By properly formulating the technical procedures for field implementation, cryogenic fracturing using liquid nitrogen could be an advantageous option for fracturing unconventional reservoirs.

In modeling of geological carbon storage, dissolution of supercritical CO2 (scCO2) is often assumed to be instantaneous with equilibrium phase partitioning. In contrast, recent core-scale imbibition experiments have shown a prolonged depletion of residual scCO2 by dissolution, implying a non-equilibrium mechanism. In this study, eight pore-scale scCO2 dissolution experiments in a 2D heterogeneous, sandstone-analog micromodel were conducted at supercritical conditions (9MPa and 40°C). The micromodel was first saturated with deionized (DI) water and drained by injecting scCO2 to establish a stable scCO2 saturation. DI water was then injected at constant flow rates after scCO2 drainage was completed. High resolution time-lapse images of scCO2 and water distributions were obtained during imbibition and dissolution, aided by a scCO2-soluble fluorescent dye introduced with scCO2 during drainage. These images were used to estimate scCO2 saturations and scCO2 depletion rates. Experimental results show that (1) a time-independent, varying number of water-flow channels are created during imbibition and later dominant dissolution by the random nature of water flow at the micromodel inlet, and (2) a time-dependent number of water-flow channels are created by coupled imbibition and dissolution following completion of dominant imbibition. The number of water-flow paths, constant or transient in nature, greatly affects the overall depletion rate of scCO2 by dissolution. The average mass fraction of dissolved CO2 (dsCO2) in water effluent varies from 0.38% to 2.72% of CO2 solubility, indicating non-equilibrium scCO2 dissolution in the millimeter-scale pore network. In general, the transient depletion rate decreases as trapped, discontinuous scCO2 bubbles and clusters within water-flow paths dissolve, then remains low with dissolution of large bypassed scCO2 clusters at their interfaces with longitudinal water flow, and finally increases with coupled transverse water flow and enhanced dissolution of large scCO2 clusters. The three stages of scCO2 depletion, common to experiments with time-independent water-flow paths, are revealed by zoom-in image analysis of individual scCO2 bubbles and clusters. The measured relative permeability of water, affected by scCO2 dissolution and bi-modal permeability, shows a non-monotonic dependence on saturation. The results for experiments with different injection rates imply that the non-equilibrium nature of scCO2 dissolution becomes less important when water flow is relatively low and the time scale for dissolution is large, and more pronounced when heterogeneity is strong.

CO2 flooding is a proven enhanced oil recovery (EOR) technique and is also considered as a potential method for CO2 sequestration. Despite having successful field trials on CO2 EOR, the effects of reservoir wettability and permeability heterogeneity on the efficiency of miscible CO2 flooding are not well understood. In this work, laboratory investigations have been carried out to evaluate the influence of these properties on the miscible CO2 EOR performance. The wettability of hydrophilic Berea core samples was altered to be oil-wet by vacuum saturation of the clean and dry core samples with n-hexadecane. The permeability heterogeneity was obtained by combining two half pieces of axially split water-wet core samples of different permeabilities. Core flooding experiments were conducted for n-hexadecane - synthetic brine - CO2 systems at 1400 psig backpressure to achieve minimum miscibility pressure (MMP) of CO2 in n-hexadecane at the test temperature (24 ± 1 °C). It was found that wettability strongly influences CO2 EOR. For the alternate cases of previously brine flooded (to remaining oil saturation) oil-wet and water-wet core samples, five pore volumes (PVs) of CO2 recovered 100% and only 43% of remaining oil in place (ROIP) respectively. Three PVs of CO2 could recover only about 0-5% ROIP from the split core samples. The mechanisms underlying these results are discussed. This study sheds light on the significant influence of reservoir wettability and permeability heterogeneity on the performance of miscible CO2 EOR.