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DOE OSTI2022

Microbial colonization and persistence in deep fractured shales is guided by metabolic exchanges and viral predation

Background: Microbial colonization of subsurface shales following hydraulic fracturing offers the opportunity to study coupled biotic and abiotic factors that impact microbial persistence in engineered deep subsurface ecosystems. Shale formations underly much of the continental USA and display geographically distinct gradients in temperature and salinity. Complementing studies performed in eastern USA shales that contain brine-like fluids, here we coupled metagenomic and metabolomic approaches to develop the first genome-level insights into ecosystem colonization and microbial community interactions in a lower-salinity, but high-temperature western USA shale formation. Results: We collected materials used during the hydraulic fracturing process (i.e., chemicals, drill muds) paired with temporal sampling of water produced from three different hydraulically fractured wells in the STACK (Sooner Trend Anadarko Basin, Canadian and Kingfisher) shale play in OK, USA. Relative to other shale formations, our metagenomic and metabolomic analyses revealed an expanded taxonomic and metabolic diversity of microorganisms that colonize and persist in fractured shales. Importantly, temporal sampling across all three hydraulic fracturing wells traced the degradation of complex polymers from the hydraulic fracturing process to the production and consumption of organic acids that support sulfate- and thiosulfate-reducing bacteria. Furthermore, we identified 5587 viral genomes and linked many of these to the dominant, colonizing microorganisms, demonstrating the key role that viral predation plays in community dynamics within this closed, engineered system. Lastly, top-side audit sampling of different source materials enabled genome-resolved source tracking, revealing the likely sources of many key colonizing and persisting taxa in these ecosystems. Conclusions: These findings highlight the importance of resource utilization and resistance to viral predation as key traits that enable specific microbial taxa to persist across fractured shale ecosystems. We also demonstrate the importance of materials used in the hydraulic fracturing process as both a source of persisting shale microorganisms and organic substrates that likely aid in sustaining the microbial community. Moreover, we showed that different physicochemical conditions (i.e., salinity, temperature) can influence the composition and functional potential of persisting microbial communities in shale ecosystems. Together, these results expand our knowledge of microbial life in deep subsurface shales and have important ramifications for management and treatment of microbial biomass in hydraulically fractured wells.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2024

Revealing complex subsurface dynamics with continuous seismic monitoring: Observations using distributed acoustic sensing and surface orbital vibrators during hydraulic fracturing

Understanding hydraulic fracturing is crucial to improving the stimulation of unconventional reservoirs and increasing fluid production. This study develops a novel seismic monitoring technology using distributed acoustic sensing (DAS) and surface orbital vibrators (SOV) to capture fracture seismic response and mechanical properties at high temporal intervals. We analyze continuous time-lapse vertical seismic profiling (VSP) data acquired every hour during the first nine days of treatment of an unconventional reservoir in the Austin Chalk/Eagle Field Laboratory. The VSP data contain clear seismic signals scattered from the activated fractures. The spatiotemporal changes of the fracture reflectivity revealed by the SOV/DAS data correlate well with the observations of fracture locations inferred from low-frequency DAS data. These results capture the fracture opening and closure processes, as well as highlight potential prestage activations of the fractures due to hydraulic connectivity with preexisting fracture systems. Therefore, analysis of the presented data set provides a unique opportunity to understand fracture initiation and subsequent evolution, not only in the context of unconventional resources but also in enhanced geothermal systems.

Correa, Julia↗

DOE OSTI2018

Natural and Hydraulic Fracture Density Prediction and Identification of Controllers

Discrete Fracture Networks (DFN’s) incorporated into hydraulic fracture modeling and reservoir simulation are typically constructed and calibrated to all available high-quality natural fracture data from image logs and core, which generally results in an extremely limited calibration data set. To extrapolate these data over large areas, more broadly sampled data sets, such as discontinuity-related 3-D seismic attributes are often used. Broad spatial trending methodologies can potentially misrepresent natural fracture systems through over-reliance on seismic attributes that are commonly influenced by noise. The Hydraulic Fracture Test Site (HFTS) provides a rare insight of the subsurface natural fracture network and controlling factors on fracture distribution from a mechanical and lithological standpoint. The physical occurrence of hydraulic fractures and their interaction and relationship to preexisting natural fractures can be predicted using analytical models. Such model outputs can be applied to provide higher confidence when developing DFN’s.

Campbell, Whitney↗

DOE OSTI2019

Thermal Transport and Fracture Behavior of Sintered Fuel Pellets: Experimental Validation of NEAMS Tool MARMOT

The project targets at experimental validation of NEAMS tool MARMOT for predicting thermal transport and fuel fracture. The key components of the project include: (1) sintering UO 2 samples with well-controlled microstructures (grain size, pore, fission bubble, porosity and pore distribution either in intra- or inter-granular pores); (2) thermal conductivity measurements of these wellcharacterized polycrystalline samples; (3) indentation testing of sintered UO 2 with various grain size, porosity and stoichiometry to obtain fracture and crack propagation mechanisms (inter or intragranular fracture); and (4) validation and uncertainty quantification of the MARMOT thermal transport and fracture models. The high quality experimental data will be used to validate the predictions of MARMOT for thermal transport and fracture, using average data and local microstructure information. In this work, UO 2 fuels with controlled microstructure (grain size, pore size/structure and fuel chemistry) were successfully prepared by high energy ball milling of the hyper-stoichiometric UO 2+x powders purchased commercially, and consolidated by spark plasma sintering. Dense nano-sized UO 2 fuel pellets with controlled stoichiometry were sintered by SPS. The effects of different SPS sintering parameters on the pore size and distribution were investigated, and the correlation among the SPS parameter – microstructure control – stoichiometry/defect structure was established. To further control the pore structure and fuel chemistry, systematic thermal annealing of the sintered fuels with the controlled pore structure was performed in a reduced. The controlled microstructure and fuel chemistry enable the investigation of the separate effects of pore structure and fuel chemistry on thermal transport behavior. The mechanical properties of the sintered UO 2 fuels were tested by nanoindentation and microindentation testing at different temperatures. The fracture behavior of the sintered fuels as functions of grain structure and temperature was investigated. Nanocrystalline UO 2 display higher hardness than microcrystalline counterpart, consistent with the Hall-Petch strengthening mechanism. Greater Young’s modulus and fracture toughness are also identified for the nanocrystalline UO 2 , and hardness and Young’s modulus decrease with temperature, suggesting better ductility of oxide fuels at greater temperature at small length scale. Hyper-stoichiometric UO 2 specimen displays higher hardness and fracture toughness than stoichiometric UO 2 , due to the impediment of the crack propagation by the oxygen interstitial atoms. These results are useful in understanding the mechanical properties of the high burn-up structure (HBS) formed in nuclear fuels during reactor operation, and also provide critical experimental data as the input for the development and validation of the MARMOT fracture model of nuclear fuels. The thermal properties of the sintered UO 2 fuel pellets with controlled grain structure, fuel chemistry and pore structures are measured by laser flash and the impact of the microstructure characteristics on the thermal transport properties is elucidated. Through a close collaboration with the MARMOT team at Idaho National Laboratory, the thermal properties of the sintered oxide fuel pellets with controlled microstructures are measured experimentally, and modeled using the developed MARMOT thermal transport models for a joint effort of demonstrating high spatial resolution measurements at the microstructural level on as-fabricated nuclear fuels and materials and obtain critical experimental data for model validation and properties predictions. In this work, we also conducted sensitivity analysis and uncertainty quantification (UQ) on a mesoscale simulation that has been applied to understand the effective thermal conductivity of UO 2 reactor fuel using the MARMOT tool. We also conduced UQ on mechanistic macroscale models that have been developed to predict the effective thermal conductivity. The most sensitive parameter is the thermal conductivity of bulk UO 2 for the thermal conductivity models. In the future, the predicted simulation distributions need to be compared to experimental data for validation of the models.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

CO 2 -Responsive Fracturing Fluids for Enhanced Geothermal Systems (Final Report)

Our group has recently developed StimuFrac, a non-toxic stimuli-responsive fracturing fluid consisting of a CO 2 -reactive polymer which has shown at the lab-scale to consistently fracture rock cores at significantly lower net pressures in a range of representative geothermal pressure/temperature conditions. However, until now the mechanism/s responsible for more effective fracturing, of critical importance to optimize fracturing performance as well as strategize injection methodologies for field deployment, was not understood. In this document, we report (1) on the two main mechanisms responsible for fracturing rock at lower net pressures with StimuFrac; (2) the phase behavior of StimuFrac/CO 2 under geothermal wellbore conditions; and (3) based on high-temperature true triaxial stimulations, detailed evidence that StimuFrac/CO 2 is the best performing stimulation fluid under EGS T/P conditions as compared to water, waterless CO 2 , and CO 2 /water fracturing fluids. This is because i) it requires significantly lower volumes of CO 2 due to its reduced leak off into the formation by the crosslinked polymer solution; ii) large fractures can be generated reproducibly at both low and high CO 2 injection flow rates, and iii) the reversible (previously reported) viscosity increase of StimuFrac could be beneficial to transport proppants when they become available for EGS. These results were particularly evident for hot nearly dry rock as well as partially and nearly fully water-saturated granitic rock. GTO requires StimuFrac to be evaluated in fully water-saturated rock to determine whether the above-described performance applies under these conditions. Since (1) GTO considers there is no enough evidence for Sa different StimuFrac formulation to work below 90C (where full water-saturation in an open system is possible) and (2) no polyaxial loading frame larger than a few centimeters that can do hydraulic fracturing tests while maintaining the rock sample fully saturated with water at 200 C exists; PNNL concludes that the only way to determine if StimuFrac represents an advanced fracturing fluid alternative for EGS, is to perform a stimulation in an actual EGS reservoir.

15 GEOTHERMAL ENERGY↗

NASA NTRS1976

A fractographic study of the edge-sliding mode in fracture toughness testing

A fractographic study of Mode II fracture surfaces has been conducted for the purpose of identifying the microstructural mechanisms responsible for fracture in the edge-sliding mode. A compact shear (CS) specimen was employed to generate the fracture surfaces and also to establish Mode II fracture toughness values for Ti-6Al-4V, A533-B steel, and several aluminum alloys. In all tests, one of the two edge cracks sustained complete Mode II fracture while the other exhibited only a limited amount of subcritical crack growth. Mode II fracture surfaces, which were unique in appearance, have been examined by optical and scanning electron microscopy. It was determined that shear (or parabolic) microvoid coalescence was the dominant mechanism for Mode II fracture. It was also established that most of the surface abrasions were created by the relative sliding of the fracture surfaces during unstable fracture rather than the crack initiation process.

Jones, D. L.↗

NASA NTRS1976

Ductile fracture theories for pressurised pipes and containers

Two mechanisms of fracture are distinguished. Plane strain fractures occur in materials which do not undergo large-scale plastic deformations prior to and during a possible fracture deformation. Plane stress or high energy fractures are generally accompanied by large inelastic deformations. Theories for analyzing plane stress are based on the concepts of critical crack opening stretch, K(R) characterization, J-integral, and plastic instability. This last is considered in some detail. The ductile fracture process involves fracture initiation followed by a stable crack growth and the onset of unstable fracture propagation. The ductile fracture propagation process may be characterized by either a multiparameter (discrete) model, or some type of a resistance curve which may be considered as a continuous model expressed graphically. These models are studied and an alternative model is also proposed for ductile fractures which cannot be modeled as progressive crack growth phenomena.

Erdogan, F.↗

NASA NTRS1977

Mechanical behavior and fracture characteristics of off-axis fiber composites. 1: Experimental investigation

The mechanical behavior, fracture surfaces, and fracture modes of unidirectional high-modulus graphite-fiber/epoxy composites subjected to off-axis tensile loads were investigated experimentally. The investigation included the generation of stress-strain-to-fracture data and scanning electron microscope studies of the fractured surfaces. The results led to the identification of fracture modes and distinct fracture surface characteristics for off-axis tensile loading. The results also led to the formulation of critical for identifying and characterizing these fracture modes and their associated fracture surfaces. The results presented and discussed herein were used in the theoretical investigation and comparisons described in Part 2. These results should also provide a good foundation for identifying, characterizing, and quantifying fracture modes in both off-axis and angle-plied laminates.

Sinclair, J. H.↗

NASA NTRS1978

Metallurgical characterization of the fracture of aluminum alloys

A systematic investigation was conducted to examine the fracture behavior of the structural aluminum alloys 2024, 6061, 7075, and 7178 (in selected heat treatments) tested under several controlled conditions. The investigation included both time independent (tensile, shear, and precracked notch-bend) fractures and time dependent (fatigue and stress corrosion) fractures. Specimens were obtained from both sheet and plate material and tested in longitudinal and transverse orientations. Strain rate effects on fracture morphology were examined in tension and shear tests. Fatigue fracture studies included an examination of the influence of minimum-to-maximum-load ratio on fracture morphology. Second-phase particles observed on fracture surfaces and metallographically prepared sections and corrosion products associated with stress corrosion fractures were analyzed chemically using scanning electron microscopy and energy-dispersive X-ray analysis. Fracture morphology was related to the microstructural features, the testing conditions, and the form of commercial product.

Bhandarkar, M. D.↗

NASA NTRS1983

Fracture behavior of the Space Shuttle thermal protection system

Stable crack-growth and fracture-toughness experiments were conducted using precracked specimens machined from LI-900 reusable surface insulation (RSI) tiles of the Space Shuttle thermal protection system (TPS) at room temperature. Similar fracture experiments were conducted on fracture specimens with preexisting cracks at the interface of the tile and the strain isolation pad (SIP). Stable crack growth was not observed in the LI-900 tile fracture specimens which had a fracture toughness of 12.0 kPa sq rt of m. The intermittent subcritical crack growth at the tile-pad interface of the fracture specimens was attributed to successive local pull-outs due to tensile overload in the LI-900 tile and cannot be characterized by linear elastic fracture mechanics. No subcritical interfacial crack growth was observed in the fracture specimens with densified LI-900 tiles where brittle fracture initiated at an interior point away from the densification.

Komine, A.↗

NASA NTRS1990

Computational simulation of structural fracture in fiber composites

A methodology was developed for the computational simulation of structural fracture in fiber composites. This methodology consists of step-by-step procedures for mixed-mode fracture in generic components and an integrated computer code, Composite Durability Structural Analysis (CODSTRAN). The generic types of composite structural fracture include: (1) single and combined mode fracture in beams; 2) laminate free-edge delamination fracture; and (3) laminate center flaw progressive fracture. Structural fracture is identified by rapid changes in one or all of the following: (1) displacements, (2) frequencies, (3) the buckling loads, or (4) the strain energy release rate. These rapid changes are herein assumed to denote imminent structural fracture. Based on these rapid changes, parameters are identified which can be used as guidelines for structural fracture, inspection intervals and retirement for cause.

Chamis, Christos C.↗

NASA NTRS1990

Computational simulation of structural fracture in fiber composites

A methodology was developed for the computational simulation of structural fracture in fiber composites. This methodology consists of step-by-step procedures for mixed mode fracture in generic components and of an integrated computer code, Composite Durability Structural Analysis (CODSTRAN). The generic types of composite structural fracture include single and combined mode fracture in beams, laminate free-edge delamination fracture, and laminate center flaw progressive fracture. Structural fracture is assessed in one or all of the following: (1) the displacements increase very rapidly; (2) the frequencies decrease very rapidly; (3) the buckling loads decrease very rapidly; or (4) the strain energy release rate increases very rapidly. These rapid changes are herein assumed to denote imminent structural fracture. Based on these rapid changes, parameters/guidelines are identified which can be used as criteria for structural fracture, inspection intervals, and retirement for cause.

Chamis, C. C.↗

NASA NTRS1993

Combined mode I and mode II fracture of monolithic ceramics

The mode I, mode II, and combined mode I-mode II fracture behaviors of a coarse-grained silicon nitride, a fine-grained silicon nitride, and an alumina were investigated. These ceramics were fractured from two types of fracture initiating flaws: small surface flaws and large single edge precracks. The small surface flaws were introduced by Knoop indentation in flexural samples at various angles to the tensile stress direction and fractured in four-point bending. The samples with large precracks were fractured in the asymmetric four-point-bend geometry. The mixed-mode fracture toughness values obtained from the two flaw configurations were in good agreement with each other. All three ceramics displayed very similar mixed-mode fracture behavior, although their microstructures were not similar. Comparison of experimental data to mixed-mode fracture theories revealed that the minimum strain energy density theory best described the mixed-mode fracture behavior of all three ceramics.

Tikare, Veena↗

NASA NTRS1994

The Relationship Between Constraint and Ductile Fracture Initiation as Defined by Micromechanical Analyses

The use of small laboratory specimens to predict the integrity of large, complex structures relies on the validity of single parameter fracture mechanics. Unfortunately, the constraint loss associated with large scale yielding, whether in a laboratory specimen because of its small size or in a structure because it contains shallow flaws loaded in tension, can cause the breakdown of classical fracture mechanics and the loss of transferability of critical, global fracture parameters. Although the issue of constraint loss can be eliminated by testing actual structural configurations, such an approach can be prohibitively costly. Hence, a methodology that can correct global fracture parameters for constraint effects is desirable. This research uses micromechanical analyses to define the relationship between global, ductile fracture initiation parameters and constraint in two specimen geometries (SECT and SECB with varying a/w ratios) and one structural geometry (circumferentially cracked pipe). Two local fracture criteria corresponding to ductile fracture micromechanisms are evaluated: a constraint-modified, critical strain criterion for void coalescence proposed by Hancock and Cowling and a critical void ratio criterion for void growth based on the Rice and Tracey model. Crack initiation is assumed to occur when the critical value in each case is reached over some critical length. The primary material of interest is A516-70, a high-hardening pressure vessel steel sensitive to constraint; however, a low-hardening structural steel that is less sensitive to constraint is also being studied. Critical values of local fracture parameters are obtained by numerical analysis and experimental testing of circumferentially notched tensile specimens of varying constraint (e.g., notch radius). These parameters are then used in conjunction with large strain, large deformation, two- and three-dimensional finite element analyses of the geometries listed above to predict crack initiation loads and to calculate the associated (critical) global fracture parameters. The loads are verified experimentally, and microscopy is used to measure pre-crack length, crack tip opening displacement (CTOD), and the amount of stable crack growth. Results for A516-70 steel indicate that the constraint-modified, critical strain criterion with a critical length approximately equal to the grain size (0.0025 inch) provides accurate predictions of crack initiation. The critical void growth criterion is shown to considerably underpredict crack initiation loads with the same critical length. The relationship between the critical value of the J-integral for ductile crack initiation and crack depth for SECT and SECB specimens has been determined using the constraint-modified, critical strain criterion, demonstrating that this micromechanical model can be used to correct in-plane constraint effects due to crack depth and bending vs. tension loading. Finally, the relationship developed for the SECT specimens is used to predict the behavior of circumferentially cracked pipe specimens.

Panontin, Tina L.↗

DOE OSTI2019

Research Considerations for Foam Fracturing in Stimulation Development for Enhanced Geothermal Systems

In regions where hydraulic fracturing is being considered for enhanced geothermal systems (EGS), and use of water is an issue, foam fracturing is an attractive option as a reduced water or waterless stimulation method. Although it has been shown to be an effective alternative in oil & gas production, foam fracturing has not yet been demonstrated in geothermal energy development. There are many challenges encountered in EGS. The reservoir may be located at great depth where earth stresses will be large and rock strength may be high. In addition, the viscosity of foam is higher than that of a pure single-phase fluid. Thus, the fracturing pressure will be increased substantially if a conventional fracturing routine is used. Moreover, fracturing in EGS systems may have more potential for induced seismicity. A proactive approach is proposed to address this technical challenge by using pulsed injection in a current project, sponsored by the U.S. DOE GTO Waterless Stimulation Initiative. This approach enables the dynamic responses of rock structure to be utilized and a new cavitation-based material-removal mechanism to be explored for enhanced fracturing efficiency. It also offers an approach to mitigate fracturing-induced seismicity and the potential to control dynamic behavior of foamed fluids. Research considerations will be described for investigation of the above phenomena in foam fracturing for EGS stimulation development.

Wang, Hong↗

DOE OSTI2019

Fracture Tracer Injection Response to Pressure Perturbations at an Injection Well

The EGS Collab project constructed an approximately ten-meter scale field site where fracture stimulation and flow/transport models can be validated against controlled, in-situ experiments. The first multi-well experimental site was established at the 4850 level of the Stanford Underground Research Facility (SURF) in the Homestake Mine located in South Dakota. Hydraulic fractures were created at an injection well drilled sub-horizontal from the drift. A flow system was established in one set of fractures by injection water at approximately 400 ml/min between a set of packers 164 feet from the drift wall in the injection well through a hydraulically stimulated fracture. Injected water was recovered from five locations in 4 nearby wells. From the end of October to the middle of November of 2018, a series of fracture characterization tests were conducted using a series of 10 tracer tests (7 which used C-dot and chloride as conservative solute tracers) to assess the flow pathway in the stimulated fracture. The injected tracers were detected in three of the five water production locations where the total water recovery ranged from approximately 50 to 80% of the injected water depending on the day the test was being conducted. Analysis of a series of tracers during this two-week period suggest a large change in the flow fracture field occurred during this testing period. A comparison of the tracer breakthrough curves at the production well showed a marked decrease in the initial and peak concentration over time, whereas the OB well exhibited an increase in the initial and peak concentration arrival during this fracture characterization testing period. These changes are believed to be in response to a number of higher-pressure short-term injections at the injection well in early November (2nd to the 6th). Results of this testing suggest that the fracture flow pathways can be altered as a result of the pressure perturbations in the injection well on the integrity of adjacent monitoring wells. Results from the EGS Collab project will support the DOE Geothermal Technology Office FORGE and other EGS development efforts.

15 GEOTHERMAL ENERGY↗

DOE OSTI2019

Multi-stage geologic fracturing

Explosive geologic fracturing methods, devices, and systems can be used in combination with other geologic fracturing means, such as hydraulic fracturing methods, devices and systems, or other fluid-based fracturing means. An exemplary method comprises introducing an explosive system into a wellbore in a geologic formation, detonating the explosive system in the wellbore to fracture at least a first portion of the geologic formation adjacent to the wellbore, and introducing pressurized fluid into the wellbore to enhance the fracturing of the first portion of the geologic formation. Such multi-stage fracturing can further enhance the resulting fracturing of geologic formation relative to explosive fracturing alone.

Mace, Jonathan Lee↗

DOE OSTI2020

Fracture toughness of zirconia with a nanometer size notch fabricated using focused ion beam milling

Zirconia with 3 mol% yttria (3Y-TZP) has been used for dental crowns and bridges due to its excellent mechanical behavior. Performing fracture toughness testing on this nanograin material, however, can be a challenge. For reliable results, fracture toughness testing requires an extremely sharp notch in the test specimen that closely approximates a very sharp crack. This study was to investigate an alternative method to produce nanometer-sized notches, which are less than the average grain size of 3Y-TZP, during the preparation of single-edge V-notched beam specimens and report the resulting fracture toughness value. We present a method using focused ion beam (FIB) milling to fabricate nanometer-sized notches in 3Y-TZP. The notch tip is <100 nm wide, which is smaller than the grain size, and is consistent throughout the thickness of the specimen. The FIB-notched specimens show a much reduced average fracture toughness of 5.64 ± 1.14 MPa√m compared to 8.90 ± 0.23 MPa√m for the specimens without FIB-notches. The FIB-milling did not appear to create any monoclinic phase prior to fracture toughness testing. Fractures originated at the FIB-notches, and the notch size can be readily identified post-mortem using a microscope. A considerable amount of tetragonal-to-monoclinic phase transformation was observed throughout the fracture surfaces. FIB milling provides an alternative method to fabricate nanometer-sized notches that are smaller than the grain size of tetragonal zirconia polycrystal. The fracture toughness determined using FIB-notches was ~5.64 MPa√m, smaller than the specimens with V-notches fabricated using saw blades.

36 MATERIALS SCIENCE↗