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DOE OSTI2020

Fundamental Understanding of Methane-Carbon Dioxide-Water (CH 4 -CO 2 - H 2 O) Interactions in Shale Nanopores under Reservoir Conditions (Quarterly Report)

Shale is characterized by the predominant presence of nanometer-scale (1-100 nm) pores. The behavior of fluids in those pores directly controls shale gas storage and release in shale matrix and ultimately the wellbore production in unconventional reservoirs. Recently, it has been recognized that a fluid confined in nanopores can behave dramatically differently from the corresponding bulk phase due to nanopore confinement. CO 2 and H 2 O, either preexisting or introduced, are two major components that coexist with shale gas (predominately CH 4 ) during hydrofracturing and gas extraction. Note that liquid or supercritical CO 2 has been suggested as an alternative fluid for subsurface fracturing such that CO 2 enhanced gas recovery can also serve as a CO 2 sequestration process. Limited data indicate that CO 2 may preferentially adsorb in nanopores (particularly those in kerogen) and therefore displace CH 4 in shale. Similarly, the presence of water moisture seems able to displace or trap CH 4 in shale matrix. Therefore, fundamental understanding of CH 4 -CO 2 -H 2 O behavior and their interactions in shale nanopores is of great importance for gas production and the related CO 2 sequestration. This project focuses on the systematic study of CH 4 -CO 2 -H 2 O interactions in shale nanopores under high-pressure and high temperature reservoir conditions. The proposed work will help develop new stimulation strategies to enable efficient resource recovery from fewer and less environmentally impactful wells.

04 OIL SHALES AND TAR SANDS↗

NASA NTRS1993

Lineament analysis and tectonic interpretation for the Tharsis region

The Tharsis region of Mars is critical to any study of Martian tectonics. This region (65 N and 65 S latitude; 45 W to 157.5 W longitude) is characterized by an asymmetrical dome-shaped topographic high approximately 8000 km across. Affecting over 25 percent of the surface area, this region has been the center of most of the major tectonic and volcanic activity that has taken place on the Martian surface. Lineament studies are the primary tool available for studying tectonic processes on terrestrial planets such as Mars. At least three major lineament systems can be delineated in the Tharsis region; north-south and east-west trending lineament systems are superimposed on an older northwest trending lineament system. Four centers of uplift have been identified based on the occurrence of radial fracture patterns. Preliminary results indicate that the formation of the Tharsis Dome may not have resulted from a single uplift event, but may instead have resulted from as many as four uplift events. The northwest trending fracture may represent a pre-existing zone of weakness which contributed to the early formation of the Tharsis Dome. The 1:2,000,000 scale photo mosaic maps of Mars were examined and lineaments were identified. The end points of each lineament were measured and recorded in an X-Y reference coordinate frame.

Anderson, Robert↗

DOE OSTI2021

Mechanical characterization of 304L-VAR stainless steel in tension with a full coverage of low, intermediate, and high strain rates

A 304L-VAR stainless steel is mechanically characterized in tension over a full range of strain rates from low, intermediate, to high using a variety of apparatuses. While low- and high-strain-rate tests are conducted with a conventional Instron and a Kolsky tension bar, the tensile tests at intermediate strain rates are conducted with a fast MTS and a Drop-Hopkinson bar. The fast MTS used in this study is able to obtain reliable tensile response at the strain rates up to 150 s -1 , whereas the lower limit for the Drop-Hopkinson bar is 100 s -1 . Combining the fast MTS and the Drop-Hopkinson bar closes the gap within the intermediate strain rate regime. Using these four apparatuses, the tensile stress-strain curves of the 304L-VAR stainless steel are obtained at strain rates on each order of magnitude ranging from 0.0001 to 2580 s -1 . All tensile stress-strain curves exhibit linear elasticity followed by significant work hardening prior to necking. After necking occurrs, the specimen load decreases, and the deformation becomes highly localized until fracture. The tensile stress-strain response of the 304L-VAR stainless steel exhibits strain rate dependence. The flow stress increases with increasing strain rate and is described with a power law. The strain-rate sensitivity is also strain-dependent, possibly due to thermosoftening caused by adiabatic heating at high strain rates. The 304L-VAR stainless steel shows significant ductility. The true strains at the onset of necking and at failure are determined. The results show that the true strains at both onset of necking and failure decrease with increasing strain rate. The true failure strains are approximately 200% at low strain rates but are significantly lower (~100%) at high strain rates. The transition of true failure strain occurs within the intermediate strain rate range between 10 -2 and 10 2 s -1 . A Boltzmann description is used to present the effect of nominal strain rate on true failure strain.

304L-VAR stainless Steel↗

DOE OSTI2024

Computed Tomography Scanning and Petrophysical Measurements of Eastern Williston Basin Twin Buttes and Hagel Formations

The computed tomography (CT) facilities and the Multi-Sensor Core Logger (MSCL) at the U.S. Department of Energy’s (DOE) National Energy Technology Laboratory (NETL) in Morgantown, West Virginia, were used to characterize core from two wells that represent coal resources across North Dakota. These include the MC23080C Well in Mercer County and the 23-B001 Well in Oliver County. The primary impetus of this work was to capture a detailed digital representation of the core from the MC23080C and 23-B001 Wells. The collaboration between the NETL and the Energy and Environment Research Center (EERC) enables other research entities to access information about this potential carbon ore, rare earth, and critical mineral resource plays in the Williston Basin. All equipment and techniques used were non-destructive, enabling future examinations and analyses to be performed on these cores. Fractures, discontinuities, and millimeter-scale features were readily detectable with the medical CT scanner acquired images. Imaging with the NETL medical CT scanner was performed on entire cores. Qualitative analysis of the medical CT images, coupled with X-ray fluorescence (XRF), gamma density, and magnetic susceptibility measurements from the MSCL were useful in identifying zones of interest for potential future analysis. Higher-resolution industrial and micro-CT images were acquired from selected zones along the depth of the core to visualize the structure in higher detail. The ability to quickly identify key areas for more detailed study with higher resolution will save time and resources in future studies. The combination of methods used provides a multi-scale analysis of the core, with the resulting macro- and micro-descriptions relevant to many subsurface energy-related examinations traditionally performed at NETL.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2025

ULTIMATE Phase I project: Development of Niobium-based alloys for Turbine Applications

Current Ni-based alloys used in turbine blade applications are operating at 1100°C which is approximately 90% of the solidus of Ni-based alloys. Further increases in temperature can be achieved only through the use of alloys with higher solidus temperatures such as refractory alloys which include Mo, Nb, W, Ta alloys. Niobium has a unique combination of physical properties that include a high melting point (2468°C), lowest density (8.57 g/cc), and the lowest modulus amongst refractory alloys, a good thermal conductivity that increases from 45 W/mK at room temperature to 62 W/mK at 1093°C, good ductility with fabricability using traditional techniques, high strength, good creep resistance, and general chemical inactivity. Hence niobium alloys offer many advantages for use at the desired temperature of 1300°C. One of the major deterrents to the use of niobium and its alloys at high temperatures is achieving good oxidation resistance. In addition, achieving balanced properties of room temperature strength, ductility, fracture toughness, high temperature strength, and creep resistance required for 1300°C operation at a density of 9 g/cm 3 is extremely challenging since the addition of W which is a potent strengthener increases the density of the alloy. This project seeks to enable the development of a tri-layered turbine blade that can operate continuously at 1300°C with the core of the turbine blade providing good creep resistance, the second layer providing improved oxidation resistance over the core layer, and the third layer being an environmental barrier providing oxidation resistance. The objective of this Phase 1 project was to use computational modeling and advanced characterization tools to develop two classes of Nb alloys which could be used as the core layer and the transition layer. The first class of alloys developed in this project was a Nb-alloy designed to serve as the turbine blade core with excellent room temperature strength, ductility, and high temperature strength and creep resistance required for 1300°C operation. These alloys were designed to contain sufficient solute solution strengthening elements (W, Mo) but constrained by the density of alloy, along with the addition of elements such as Zr, Hf, Ta, C, and N to achieve a combination of primary and secondary carbide precipitation. A total of 38 “creep-resistant” alloys were designed and cast during the duration of the project. Processing techniques were developed to keep the oxygen contents as low as possible with typical oxygen contents less than 250 ppm. One alloy with a density of < 9.5 g/cc was successful in meeting the Phase 2 intermediate project mechanical property milestone requirements of room temperature ductility greater than 1.0%, 1200°C creep strain of less than 3% at 150 MPa and 100 hours in vacuum, and with solidus temperature greater than 1500ᵒC. The second class of alloys was designed to be a Nb-rich alloy with improved oxidation resistance when compared to the core layer and was designed specifically to be compatible with the core layer and the outer environmental barrier coating. This Nb- alloy will be specifically designed to be microstructurally stable at these temperatures when in contact with the core alloy and provide protection against catastrophic failure of the barrier coating. Two alloys were cast and processed but further development was discontinued to focus on the development of the creep resistant alloy.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Development of Niobium-based alloys for Turbine Applications: 20/CJ000/08/09 (ULTIMATE Phase I project)

36 MATERIALS SCIENCE↗

NASA NTRS1974

Role of HF and Zr in the hydrogen embrittlement of Ta and Cb alloys

An attempt is made to characterize the hydrogen embrittlement of aged T-111 and similar Ta and Cb alloys and to describe the mechanisms believed responsible for the increased sensitivity of T-111 to low temperature hydrogen embrittlement after aging for 1000 hr or longer near 1040 C. A total of eight Ta-base alloys and two Cb-base alloys were investigated. The effects of pre-age annealing temperature, aging time, temperature and environment, and alloy composition on the susceptibility to hydrogen embrittlement were investigated. The primary method of determining the effects of these variables on the ductility of T-111 was by bend testing at 25 and -196 C. Fractured specimens were examined by the scanning electron microscope, electron microprobe, metallography, and X-ray diffraction.

Stephens, J. R.↗

NASA NTRS2022

Geological, Multispectral, and Meteorological Imaging Results from the Mars 2020 Perseverance Rover in Jezero Crater

Perseverance’s Mastcam-Z instrument provides high-resolution stereo and multispectral images with a unique combination of spatial resolution, spatial coverage, and wavelength coverage along the rover’s traverse in Jezero crater, Mars. Images reveal rocks consistent with an igneous (including volcanic and/or volcaniclastic) and/or impactite origin and limited aqueous alteration, including polygonally fractured rocks with weathered coatings; massive boulder-forming bedrock consisting of mafic silicates, ferric oxides, and/or iron-bearing alteration minerals; and coarsely layered outcrops dominated by olivine. Pyroxene dominates the iron-bearing mineralogy in the fine-grained regolith, while olivine dominates the coarse-grained regolith. Solar and atmospheric imaging observations show significant intra- and intersol variations in dust optical depth and water ice clouds, as well as unique examples of boundary layer vortex action from both natural (dust devil) and Ingenuity helicopter–induced dust lifting. High-resolution stereo imaging also provides geologic context for rover operations, other instrument observations, and sample selection, characterization, and confirmation.

Mars 2020↗

DOE OSTI2022

Graphene nanoplatelets reinforced cement as a solution to leaky wellbores reinforcing weak points in hydrated Portland cement with graphene nanoparticles improves mechanical and chemical durability of wellbore cements

In this work, to improve the performance of wellbore cement under subsurface environments, graphene nanoplatelets (GNPs) were added in various percentages to Class-H cement slurry. Microstructural characterization of cement slurries cured at 90 °C and 95% RH indicates that GNP modifies the microstructure of hydrated cement by reinforcing pore spaces. As a result, the mechanical properties, such as Young's modulus and axial peak stress, obtained from high temperature triaxial compression tests are significantly improved based on different percentages of added GNPs. Furthermore, the hydrated 1 × 2 inch GNP- Portland cement cores tested under simulated deep wellbore conditions of high-temperature and high pressure (HTHP), appear to have a ductile-like behavior, when compared to a typical brittle nature of Portland cement pastes. From our observations and published data on graphene resistance to fracture, GNP addition to cement is evidently enhancing the flexibility of cement. These improvements would reduce the risks associated with wellbore cement deterioration and a consequent leakage in fossil fuel production, geothermal energy production, CO 2 storage as well as long-term sealing materials in plugging and abandonment of all wellbores at the end of their service life.

36 MATERIALS SCIENCE↗

NASA NTRS1984

Space Radiation Effects on Graphite-Epoxy Composite Materials

Radiation effects on engineering properties, dimensional stability, and chemistry on state of the art composite systems were characterized. T300/934 graphite-epoxy composite was subjected to 1.0 MeV electron radiation for a total dose of 1.0 x 10(10) rads at a rate of 5.0 x 10(7) rads/hour. This simulates a worst case exposure equivalent to 30 years in space. Mechanical testing was performed on he 4-ply unidirectional laminates over the temperature range of -250 F (116K) to +250 F (394K). A complete set of in-plane tensile elastic and strength properties were obtained (E sub 1, E sub 2, nu sub 12, G sub 12, X sub T, Y sub T, and S). In addition electron microscopy was used to study and analyze the fracture surfaces of all specimens tested. Results indicate that little difference in properties is noted at room temperature, but significant differences are observed at both low and elevated temperatures.

Milkovich, S. M.↗

NASA NTRS2004

Development and Testing of Ceramic Thermal Barrier Coatings

Ceramic thermal barrier coatings will play an increasingly important role in future gas turbine engines because of their ability to effectively protect the engine components and further raise engine temperatures. Durability of the coating systems remains a critical issue with the ever-increasing temperature requirements. Thermal conductivity increase and coating degradation due to sintering and phase changes are known to be detrimental to coating performance. There is a need to characterize the coating behavior and temperature limits, in order to potentially take full advantage of the current coating capability, and also accurately assess the benefit gained from advanced coating development. In this study, thermal conductivity behavior and cyclic durability of plasma-sprayed ZrO2-8wt%Y2O3 thermal barrier coatings were evaluated under laser heat-flux simulated high temperature, large thermal gradient and thermal cycling conditions. The coating degradation and failure processes were assessed by real-time monitoring of the coating thermal conductivity under the test conditions. The ceramic coating crack propagation driving forces and resulting failure modes will be discussed in light of high temperature mechanical fatigue and fracture testing results.

Zhu, Dongming↗

DOE OSTI2020

Size-dependent stochastic tensile properties in additively manufactured 316L stainless steel

Recent work in metal additive manufacturing (AM) suggests that mechanical properties may vary with feature size; however, these studies do not provide a statistically robust description of this phenomenon, nor do they provide a clear causal mechanism. Because of the huge design freedom afforded by 3D printing, AM parts typically contain a range of feature sizes, with particular interest in smaller features, so the size effect must be well understood in order to make informed design decisions. This work investigates the effect of feature size on the stochastic mechanical performance of laser powder bed fusion tensile specimens. A high-throughput tensile testing method was used to characterize the effect of specimen size on strength, elastic modulus and elongation in a statistically meaningful way. The effective yield strength, ultimate tensile strength and modulus decreased strongly with decreasing specimen size: all three properties were reduced by nearly a factor of two as feature dimensions were scaled down from 6.25 mm to 0.4 mm. Hardness and microstructural observations indicate that this size dependence was not due to an intrinsic change in material properties, but instead the effects of surface roughness on the geometry of the specimens. Finite element analysis using explicit representations of surface topography shows the critical role surface features play in creating stress concentrations that trigger deformation and subsequent fracture. The experimental and finite element results provide the tools needed to make corrections in the design process to more accurately predict the performance of AM components.

316L stainless steel↗

NASA NTRS2016

Evaluation of the Effect of Surface Finish on High-Cycle Fatigue for SLM-IN718

A high-cycle fatigue (HCF) knockdown factor was estimated for Inconel 718, manufactured with the selective laser melt (SLM) process. This factor is the reduction at a common fatigue life from the maximum stress in fatigue for low-stress ground (LSG) specimens to the maximum stress of those left with the original surface condition. Various vendors provided specimens. To reduce the number of degrees-of-freedom, only one heat treat condition was evaluated. Testing temperatures included room temperature, 800F, 1000F, and 1200F. The two surface conditions were compared at constant lives, where data was available. The recommended knockdown factor of the as-built surface condition (average roughness of approximately 245 micro-inches/inch) versus low-stress ground condition (roughness <= 4 micro-inches/inch) is approximately 1/3 or 33%. This is to say that for the as-built surface condition, a maximum stress of 2/3 of the stress for LSG can be expected to produce the same life in the as built surface condition. As an alternative method, the surface finish was incorporated into a new parameter with the maximum stress. The new parameter was formulated to be similar to the fracture mechanics stress intensity factor, and it was named the pseudo stress intensity factor, Kp. Using Kp, the variance seemed acceptable across all sources, and the knockdown factor was estimated over the range of data identified by Kp where data occurred. A plot of the results suggests that the knockdown factor is a function of temperature, and that for low lives the knockdown is greater than the knockdown observed above about one million cycles, where it stabilizes. One data point at room temperature was clearly different, and the sparsity of data in the higher life region reduces the value of these results. The method does appear to provide useful results, and further characterization of the method is suggested.

Lambert, Dennis M.↗

DOE OSTI2021

Micro-mechanical investigation of the thermo-mechanical properties of micro-architectured tungsten coatings

The thermo-mechanical response of micro-architectured tungsten coatings is characterized in the temperature range of 293 to 673 K using both in situ micro-compression experiments inside a scanning electron microscope (SEM) as well as image-based crystal plasticity finite element method (CPFEM) simulations. The experiments were conducted on micropillar-like specimens that were focus ion beam milled into the coatings, while the simulations were conducted on columnar-grained micropillar simulation cells constructed based on the statistics of the coating’s microstructure. The experimental results show that the stress–strain response and deformation mode exhibit a strong temperature-dependence. At room temperature, catastrophic failure is observed shortly after yield and is manifested in the form of intergranular fracture and buckling of individual columnar grains. With increasing temperature, this catastrophic failure is gradually suppressed and the material exhibits a steadier strain hardening response at 693 K. The CPFEM simulations are also shown to be in good agreement with the experimental results, and these simulations indicate that the material response is strongly influenced by the local crystallographic anisotropy and microstructure inhomogeneity. Furthermore, the simulations capture the underlying mechanisms that control the temperature-dependent transition in deformation mode. The current results highlight that the micro-architectured microstructure offers a great combination of excellent mechanical strength and structural integrity at elevated temperatures, which is of importance for high temperature applications.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Mechanical Performance of Additively Manufactured ODS 316L and 316H Stainless Steels

This work package within the Advanced Materials and Manufacturing Technologies (AMMT) program focused on the mechanical and microstructural characterization of oxide dispersion strengthened (ODS) stainless steels produced using advanced manufacturing techniques. The research aimed to identify an accelerated development path for ODS alloys by integrating additive manufacturing (AM) technologies with recent advancements in ODS materials and traditional manufacturing methods. For FY 24, the research specifically targeted exploring an accelerated development path for ODS alloys by combining AM technologies with these advancements. Novel AM and post-build processing routes were developed for ODS austenitic alloys, including Fe-Cr-Ni alloys such as 316L and 316H. Electron microscopy and mechanical characterizations were conducted to evaluate the impact of process variables on microstructure and properties, with the goal of optimizing these properties economically. Traditionally, producing ODS alloys involves multi-day, high-energy mechanical milling of alloy powder with yttria powder, followed by milled-powder consolidation through extrusion or other methods, and additional thermomechanical processing (TMP) for property control. To overcome the challenges associated with this complex and costly approach, we propose exploring alternative, cost-effective processing routes that emphasize AM and traditional TMP methods. The new processing routes for ODS alloys have achieved significantly higher strengths—several times greater than those of wrought stainless steels—while maintaining substantial ductility and fracture toughness. This report outlines the novel and economical AM-based processing routes for ODS austenitic alloys, combined with post-build TMPs, and discusses the mechanical and microstructural characteristics of the developed materials.

36 MATERIALS SCIENCE↗

NASA NTRS1992

An evaluation of mixed-mode delamination failure criteria

Many different failure criteria have been suggested for mixed mode delamination toughness, but few sets of mixed mode data exist that are consistent over the full mode I opening to mode II shear load range. The mixed mode bending (MMB) test was used to measure the delamination toughness of a brittle epoxy composite, a state of the art toughened epoxy composite, and a tough thermoplastic composite over the full mixed mode range. To gain insight into the different failure responses of the different materials, the delamination fracture surfaces were also examined. An evaluation of several failure criteria which have been reported in the literature was performed, and the range of responses modeled by each criterion was analyzed. A new bilinear failure criterion was analyzed. A new bilinear failure criterion was developed based on a change in the failure mechanism observed from the delamination surfaces. The different criteria were compared to the failure criterion. The failure response of the tough thermoplastic composite could be modeled well with the bilinear criterion but could also be modeled with the more simple linear failure criterion. Since the materials differed in their mixed mode failure response, mixed mode delamination testing will be needed to characterize a composite material. A critical evaluation is provided of the mixed mode failure criteria and should provide general guidance for selecting an appropriate criterion for other materials.

Reeder, J. R.↗

DOE OSTI2021

Machine learning to identify geologic factors associated with production in geothermal fields: A casestudy using 3D geologic data, Brady geothermal field, Nevada

In this paper, we present an analysis using unsupervised machine learning (ML) to identify the key geologic factors that contribute to the geothermal production in the Brady geothermal field. Brady is a hydrothermal system in northwestern Nevada that supports both electricity production and direct use of hydrothermal fluids. Transmissive fluid flow pathways are relatively rare in the subsurface but are critical components of hydrothermal systems like Brady and many other types of fluid flow systems in fractured rock. The ML method, non-negative matrix factorization with k-means clustering (NMFk), is applied to a library of fourteen 3D geologic characteristics hypothesized to control hydrothermal circulation in the Brady geothermal field. Our results indicate the macro-scale faults and a local step-over in the fault system preferentially occur along with production wells when compared to injection wells and non-productive wells. We infer that these are the key geologic characteristics that control the through-going hydrothermal transmission pathways at Brady. Our results demonstrate 1) the specific geologic controls on the Brady hydrothermal system and 2) the efficacy of pairing ML techniques with 3D geologic characterization to enhance the understanding of subsurface processes.

15 GEOTHERMAL ENERGY↗

NASA NTRS1997

Application of the Pseudo Wigner-Ville Distribution to the Measurement of the Dispersion of Lamb Modes in Graphite/Epoxy Plates

Acoustic waves propagate in thin plates as guided or Lamb modes. The velocities of these modes are dispersive in that they depend not only on the material elastic properties and density, but also on the frequency. Accurate characterization of Lamb wave dispersion is important in many acoustic based nondestructive evaluation techniques. It is necessary for ultrasonic measurements in thin plates to determine elastic properties and for flaw detection and localization. In acoustic emission (AE) testing, if not taken into account, highly dispersive Lamb mode propagation can lead to large errors in source location. In this study, the pseudo Wigner-Ville distribution (PWVD) was used for measurement of group velocity dispersion of Lamb waves in a unidirectional graphite/epoxy (AS4/3502) laminate. The PWVD is one of a number of transforms which provide a time-frequency representation of a digitized time series. Broad band acoustic waves were generated by a pencil lead fracture (Hsu-Neilsen source) and were detected with broad band ultrasonic transducers. The arrival times for the lowest order symmetric (S(sub 0)) and antisymmetric (A(sub 0)) Lamb modes were determined from measurements of the time at which the respective peak amplitudes occurred in the PWVD. Measurements were made at several source-to-detector distances and a least squares fit used to calculate the velocity. Results are presented for propagation along, and perpendicular to, the fiber direction. Theoretical dispersion curves were also calculated and a comparison between theory and experiment demonstrates good agreement.

Prosser, W. H.↗