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DOE OSTI2020

Self-Assembly of Silica Nanoparticles at Water–Hydrocarbon Interfaces: Insights from In Operando Small-Angle X-ray Scattering Measurements and Molecular Dynamics Simulations

To achieve tunable controls on the interactions of siliceous materials in subsurface environments bearing water and hydrocarbons, it is essential to determine the influence of hydrocarbon–water interfaces on the self-assembly of the silica particles. The hydrophilic silica particle have a tendency to aggregate on the water front of the interface. Self-assembly of silica nanoparticles proceeds via the migration of these nanoparticles to the water–hydrocarbon interface followed by aggregation at the interface. Fractal-like morphologies of assembled silica nanoparticles at water–hydrocarbon interfaces are observed. Rapid assembly of the hydrophilic silica nanoparticles at water–hydrocarbon interfaces corresponds to an overall reduction in the surface tension of water–toluene and water–heptane systems. These studies demonstrate the silica aggregation that is the precursor of silica polymerization, or nucleation and growth is influenced by the presence of hydrocarbons in subsurface geologic environments. These insights were derived from in operando ultrasmall and small-angle X-ray scattering (USAXS/SAXS) measurements, cryo-scanning electron microscopy (Cryo-SEM) imaging, and classical molecular dynamics simulations. As a result, these studies are intended to inform current and future efforts aimed at tuning silica reactivity in subsurface geologic environments to enhance permeability, the design and use of silica-based proppants to enhance fractures, and the development of effective strategies to control silica-based scaling behavior in subsurface reservoirs.

42 ENGINEERING↗

DOE OSTI2024

Large-Volume Stimulation of Rock for Greatly Enhanced Fluids Recovery using Targeted Seismic-Assisted Hydraulic Fracturing (Final Technical Report)

This project has developed and demonstrated a new technology for large-volume and targeted comminution of rock in low permeability formations to enhance recovery from unconventional oil and gas (UOG) resources. The technology is based on a strategically designed interaction of multiple induced seismic pulses that assist the hydraulic fracturing process to enhance shear and multi-planar crack formation. This greatly increased rock stimulation, through bulk comminution, is expected to cause significant increase in permeability leading to enhancement of recovery factors for sub- surface fluids. The proposed technology is especially applicable for enhanced recovery in emerging UOG plays, such as ductile shales that are resistant to opening-mode fracturing by conventional hydraulic fracturing processes. The project combines an integrated experimental and computation approach to develop and demonstrate a modular technology that can be easily implement in the field to augment current practices. The effort integrates a fundamental scientific understanding of dynamic material response under constraint and damage-induced permeability and porosity enhancements at multiple length scales, along with models of comminution due to the local release of kinetic energy associated with high shear strain rate of dynamic deformation. The results will be validated through small-scale experiments and then implemented in a lab-scale field test to demonstrate the developed technology. The project involves collaboration between a solid mechanician, a materials scientist, and a petroleum engineering geo-mechanician. It builds on a successful history of success and collaboration that includes both fundamental scientific exploration and technology development.

04 OIL SHALES AND TAR SANDS↗

NASA NTRS2001

Thermal Fatigue and Fracture Behavior of Ceramic Thermal Barrier Coatings

Thermal fatigue and fracture behavior of plasma-sprayed ceramic thermal barrier coatings has been investigated under high heat flux and thermal cyclic conditions. The coating crack propagation is studied under laser heat flux cyclic thermal loading, and is correlated with dynamic fatigue and strength test results. The coating stress response and inelasticity, fatigue and creep interactions, and interface damage mechanisms during dynamic thermal fatigue processes are emphasized.

Zhu, Dong-Ming↗

DOE OSTI2024

Enhancing Mechanical Properties of a Medium-Entropy Alloy by Regulating Mo Addition

Some multi-principal element alloys (MPEAs), including equiatomic, single-phase CrCoNi and CrCoFeMnNi are now widely recognized for their remarkable combinations of pronounced hardening rates, high ductility, and exceptional fracture toughness at room and cryogenic temperatures. To push the limit of hardenability of the medium-entropy alloy, the strategies associated with local lattice distortion or stacking fault energy (SFE) reduction that promote complex heterogeneity and defect dynamics require further investigation. The purposes of this study are to (1) further enhance the mechanical properties of a typical medium-entropy NiCoCr with alloying Mo, and (2) understand the strengthening mechanism of a Mo-added medium-entropy alloys.

Hung, Chang-Yu↗

DOE OSTI2023

Effect of an oxide layer on high velocity impact of tantalum particles characterized using molecular dynamics

Micro-cold spray, also commonly referred to as the aerosol deposition method or vacuum kinetic spraying, is a process for depositing nanostructured films of metals and ceramics by impacting solid nanoparticles at high velocity onto a substrate at room temperature and at low pressures. Tantalum films deposited by micro-cold spray are desirable because tantalum is non-reactive to certain molten metals and can therefore serve as a non-reactive barrier coating. However, unlike most other metals deposited by micro-cold spray, tantalum quickly forms an oxide layer when exposed to air. In the deposition of films using traditional cold spray with much larger particles, native oxides must fracture for particle–substrate bonding to occur. Furthermore, the fraction of the particle that is oxidized in micro-cold spray and the strain rates experienced by the particles upon impact are both much larger than in cold spray, suggesting that the role of the oxide on film deposition may be distinct. The effect of this oxide layer on particle deformation and adherence to a substrate under high strain rates is studied using molecular dynamics simulations. The effect of oxide layer thickness, particle diameter, and impact velocity are examined.

42 ENGINEERING↗

DOE OSTI2022

High Performance Circuit Pastes for Solid Oxide Fuel Cell Applications: Final Technical Report

Using a combination of in-plane electrical conductivity measurements, electrical contact resistance measurements, tensile fracture tests, double shear lap fracture tests, rapid thermal cycling adhesion tests, in situ wetting angle measurements, 3D X-ray tomography, reduction-oxidation (RedOx) cycling, scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDAX), Density Functional Theory (DFT) modeling, Molecular Dynamics (MD) modeling, and Phase Field modeling, this project determined that a new brazing technique developed by the PIs (specifically the use of nickel particles to direct the wetting and spreading of molten silver) could be used to produce well-adhered, >97% dense, electrically-conductive circuits, current collectors, and/or electrical contacts on a variety of ceramic and ceramic-coated substrates (specifically lanthanum strontium manganite, yttria stabilized zirconia, sapphire, Cr2O3-passivated stainless steel, and Al2O3-passivated stainless steel). Compared to other silver-based alternatives, Ag:Ni led to less manufacturing defects and was more tolerant of the extreme environments (isothermal high-temperature aging) and occasional abuse (rapid thermal cycling and RedOx cycling) encountered during Solid Oxide Fuel Cell and/or Solid Oxide Electrolysis Cell operation. Further, in some situations (such as when to produce Ag:Ni electrical contacts to Al2O3-protected stainless steel) the Ni particles also improved operation by acting as chemical getters that removed electrically-insulating, surface-segregating substrate impurities (i.e. by lowering the contact resistance with the underlying substrate).

36 MATERIALS SCIENCE↗

NASA NTRS1993

The Stickney impact of Phobos - A dynamical model

The hypervelocity impact that excavated the Stickney crater on Phobos is numerically modeled in order to understand the effects this collision had on the interior and surface of Phobos. The model assumes homogeneity prior to impact based on Fujiwara's (1991) results. Constitutive relations for water ice and basalt are applied in tandem models. Fracture energetics is used to show that the impact itself is sufficient to cause the cracks observed on Phobos. It is further shown that the Stickney impact itself could not have created large voids; thus, the low density of Phobos must either be compositional in nature or else the result of porosity at a scale sufficiently small to avoid scattering the impact energy substantially.

Asphaug, E.↗

DOE OSTI2024

Mechanical properties and deformation mechanisms of single crystal Mg micropillars subjected to high-strain-rate C-axis compression

Here, the mechanical properties and deformation mechanisms of single crystal magnesium under c-axis quasi-static and high-strain rate compressions are investigated through in situ scanning electron microscope (SEM) experiments and post-mortem transmission electron microscope (TEM) characterization. The findings revealed that ductility and high rates of hardening are preserved for pillars as large as 15 μm. Furthermore, rate effects result in a mild increase in flow stress with plastic deformations controlled primarily by the slip of type dislocations. Importantly and in contrast to other literature reports, plastic deformation occurs in the absence of twining. As the strain increases and plastic deformation exceeds about 4%, crystal rotation activates basal slip, <$\mathrm{a}$> type dislocations, resulting in a more rate independent flow stress. TEM observation on micropillars compressed at a strain rate of 250/s, revealed the activation of {${11}$$\bar{2}$$\bar{2}$} < $\bar{1}$$\bar{1}23$ > slip systems and high mobility of screw dislocations as major contributors to plastic strains in excess of 10% without fracture. These findings are relevant to the design of lightweight materials used in transportation systems, e.g., selection of material grain size. Moreover, the experimental data here reported provides the materials science community with a unique opportunity to validate discrete dislocation dynamics (DDD) formulations employed in multiscale design of materials.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Textile-Grade Carbon Fiber-Reinforced Polycarbonate Composites: Effect of Epoxy Sizing

In this work, epoxy-sized textile-grade polyacrylonitrile (PAN) carbon fiber (TCF) with 450 K filaments (CFTF, ORNL) was reinforced in the polycarbonate (PC) matrix using a compression molding technique. The epoxy sizing effect on the surface, thermal, and mechanical properties of TCF–PC was investigated. X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy results of the TCF–PC composite show the absence of an oxirane group (epoxy-sized TCF), which suggests a covalent bond formation between the oxirane ring and carbonyl groups from TCF and PC. Dynamic mechanical analysis results confirm a strong immobilized interface (b > 1) present between TCF and PC. The tensile, flexure, compression, and interlaminar shear strength of TCF–PC composites were 323 ± 53, 371 ± 31, 397 ± 87, and 36 ± 3 MPa, correspondingly. The fracture analysis through scanning electron microscopy shows good wettability between TCF and the PC matrix which validates the results obtained from surface and thermal characterization.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Tailoring Mechanical Properties of a Multi-Principle-Element Alloy by a Multi-Length-Scale Approach

A multiscale strengthening approach was employed to tailor the mechanical properties of a NiCoCr-based multi-principal element alloy (MPEA). Initially, the addition of Mo was utilized to strengthen the alloys by achieving grain size refinement, severe lattice distortion, and a reduction in stacking fault energy (SFE). Subsequently, the Suzuki segregation phenomenon was leveraged by carefully controlling stacking fault (SF) density via pre-straining and a subsequent 500°C heat treatment. Consequently, the Mo-added MPE alloys that were pre-strained and subsequently heat-treated exhibited a true yield stress of 2.3 GPa, with a corresponding fracture elongation of 12%. The Mo promotes complex SF interactions and the SFs formed during prior straining serve as sites for Suzuki segregation during subsequent heat treatment, varying the local SFE with Cr segregation, creating a roughened landscape and hindering dislocation dynamics. This multiscale strengthening approach presents a promising route for achieving desired mechanical properties in MPEAs.

mechanical properties↗

NASA NTRS1973

On the breakup of tectonic plates by polar wandering

The observed boundary system of the major tectonic plates on the surface of the earth lends fresh support to the hypothesis of polar wandering. A dynamic model of the outer shell of the earth under the influence of polar shift is developed. The analysis falls into two parts: (1) deriving equations for stresses caused by polar shifting; and (2) deducing the pattern according to which the fracture of the shell can be expected. For stress analysis, the theory of plates and shells is the dominant feature of this model. In order to determine the fracture pattern, the existence of a mathematical theorem of plasticity is recalled: it says that the plastic flow begins to occur when a function in terms of the differences of the three principal stresses surpasses a certain critical value. By introducing the figures for the geophysical constants, this model generates stresses which could produce an initial break in the lithosphere.

Liu, H. S.↗

DOE OSTI2021

Coupling dynamic in situ X-ray micro-imaging and indentation: A novel approach to evaluate micromechanics applied to oil shale

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. Here we show 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.)

04 OIL SHALES AND TAR SANDS↗

DOE OSTI2021

A Self-Healable Sulfide/Polymer Composite Electrolyte for Long-Life, Low-Lithium-Excess Lithium-Metal Batteries

Solid electrolyte-protected lithium-metal anodes promise energy-dense, safe cells. While sulfide solid electrolytes enable facile processability and fast ion transport, they suffer from complex chemo-mechanical issues, including Li plating-induced fracture and Li stripping-induced contact loss. To address these issues, a grafting approach is implemented to functionalize the sulfide solid electrolyte (Li 3,85 Sn 0.85 Sb 0.15 S 4 ) with a self-healing unit. This leads to a dynamic bonding between the solid electrolyte network and a mechanically robust polymer scaffold, which reversibly accommodates the volume changes of the lithium-metal anode. Thus, the approach improves the interfacial contact between the lithium-metal anode and the composite electrolyte, enabling stable cycling at a mild stack pressure (160 kPa). With a negative to positive capacity ratio equals to 1, pouch full cells with a high-nickel cathode (nickel content > 90%) and lithium-metal anode display 92% capacity retention for 140 cycles. Engineering the interface between solid electrolyte and the polymeric binder offers a promising pathway to address the chemo-mechanical issues.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Inference of phase field fracture models

The phase field approach to modeling fracture uses a diffuse damage field to represent cracks. This representation mollifies singularities that arise in computations with sharp interface models and some of the resultant difficulties in the mathematical and numerical treatment of fracture. Phase field fracture models have proven effective at representing crack propagation, branching, and merging. Specific formulations, beginning with brittle fracture, have also been shown to converge to classical solutions. Extensions to cover the range of material failure, including ductile and cohesive fracture, lead to an array of possible models. There exists a large body of literature focusing on this class of models and on the impact of model form on the predicted crack evolution. However, there have not been systematic studies into how optimal models may be chosen. Here, we take a first step in this direction by developing formal methods for identification of the best parsimonious model of phase field fracture given full-field data on the damage and deformation fields. We consider some of the main models that have been used for the degradation of elastic response due to damage and its propagation. Our approach builds upon Variational System Identification (VSI), a weak form variant of the Sparse Identification of Nonlinear Dynamics (SINDy). Furthermore, in this first communication we focus on synthetically generated data but we also consider central issues associated with the use of experimental full-field data, such as data sparsity and noise.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2021

Columnar Grain-driven Plasticity and Cracking in Nanotwinned FCC Metals

The mechanisms of strengthening and plasticity in columnar-grained metals with preferentially oriented nano-sized twins have been examined traditionally by considering dislocation processes, but rarely from the perspective of grain boundary (GB) deformation. Here, the effects of GB strain accommodation on plastic deformation in four different columnar-grained nanocrystalline nanotwinned (nt) face-centered-cubic metals (Cu, Ag, Al, and Ni) were studied by large-scale molecular dynamics simulations. It is observed that in tensile deformation parallel to coherent twin boundaries (CTBs), the dislocation mechanisms in each metal are identical and associated with GB emissions of jog and threading dislocations at small and large CTB spacings, respectively. However, CTB strengthening effects are increasingly more pronounced in columnar-grained nt metals as their shear modulus increases, which is rationalized by the dependence of GB stress concentrations on twin size, metal type and strain rate. Also, while flow stresses in nt-Cu, nt-Ag, and nt-Al metals increase linearly with decreasing CTB spacing, a maximum strength limit is reached in nt-Ni below a critical CTB spacing of 6 nm. The strength limit in nt-Ni results from columnar GB cracking induced by prominent GB sliding. For columnar-grained microstructures, GB sliding is equivalent in nt-Ag and nt-Al and slightly lower in nt-Cu but markedly higher in nt-Ni. These findings underscore the importance of new GB deformation mechanisms on plasticity and fracture in columnar-grained nt metals and enrich our understanding of CTB strengthening in fcc metals synthesized in the literature.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Effect of aging on failure mechanism of Alloy 709 at various temperatures

Alloy 709 is a novel austenitic stainless steel with high temperature creep strength, weldability, and corrosion resistance. These properties make the material suitable for applications in the structure of next-generation nuclear power plants. Enduring high temperatures for an extended period of time in the harsh environments of a nuclear power plant results in thermal aging of the material. Therefore, it is imperative to study the effect of thermal aging on the microstructure and mechanical properties of Alloy 709 before its application in the next generation power plants. In this study, hot-processed (forged + rolled), annealed and quenched ingots of Alloy 709 are aged at 650 °C for 2000 h in air and then tested at various temperatures up to 850 °C in an in-situ heating-loading Scanning Electron Microscope (SEM) equipped with Energy Dispersive Spectroscopy (EDS) and Electron Backscatter Diffraction (EBSD). The effect of testing temperature and aging on microstructural evolutions during tensile testing of as-received and aged samples are studied. Furthermore, both as-received and aged samples displayed serrations and drop in ductility at elevated temperatures, due to the effect of dynamic strain aging (DSA). The occurrence of DSA activity was found within temperatures range of 500 °C–750 °C in as-received and 550 °C - 650 °C in aged samples. The aged samples showed less elongation accompanied by shallower dimples on the fractured surface, indicating less ductile failure mechanism compared to as-received samples. Failure mechanism observations on the fracture surface using SEM fractography are correlated to the observations made on the sample surface using in-situ SEM to achieve a complementary set of information to better understand the failure mechanism of this novel alloy.

36 MATERIALS SCIENCE↗

DOE OSTI2021

A workflow to assess the efficacy of brine extraction for managing injection-induced seismicity potential using data from a CO 2 injection site near Decatur, Illinois

Injection of CO 2 for storage in a geologic formation increases pore pressure and alters in situ stresses. Depending on the orientation of any existing fault and fracture planes, such as critically stressed planes, this stress alteration will modify normal stresses acting on planes and could result in frictional sliding and release stored energy in the form of seismicity. Brine extraction (BE) is a technique that can be applied prior to, or during, CO 2 injection to reduce pore pressure for increasing storage capacity and, potentially, for reducing the likelihood of frictional sliding. Here a workflow is described to assess the efficacy of BE for mitigating frictional sliding (i.e., seismicity) during injection and entails: site characterization, stress calculations and failure assessment, static and dynamic modeling, and BE operational planning. Site characterization describes the stress field used to calculate the Coulomb Failure Function (CFF) that constrains allowable pore pressure changes and injection rates in the numerical simulation of CO 2 injection scenarios. The inclusion of BE in the workflow allows for determination of the potential need for pressure reduction, and evaluation of the effectiveness of this operation. Example application of the workflow using an injection field dataset near Decatur, IL, provides insight on fracture planes and stresses at the site, formation properties and the impact of variable CO 2 injection-rate targets on whether BE plans are required. The study workflow indicates that BE could enhance CO 2 injection rate by 39% and correspondingly reduce the potential for injection-induced seismicity as indicated by a reduction in CFF.

58 GEOSCIENCES↗

DOE OSTI2022

Leakoff assessment of nanoparticle-stabilized CO 2 foams for fracturing applications

The leakoff of multiphase systems through porous media is a complicated process. In this study, we have designed an experimental setup that is used to assess the leakoff of the liquid and gas phase under pressurized conditions. The novelty of this study is that while most previous studies utilized fluid/gas in the aqueous phase, nanoparticles are introduced in this study, which formed a solid/fluid/gas multiphase system to boost foam performance and reduce leakoff. In the parametric experimental analysis, the effects of foam quality, core permeability, surfactant concentration, and polymer concentration on the dynamic and static leakoff rates of liquid and gas are evaluated. It was found that core permeability affects the leakoff of foam the most with a leakoff coefficient of up to 1.37015 $ft/\sqrt{min}$ for gas and up to 0.1056 $ft/\sqrt{min}$ for liquid under the experiment settings herein. The leakoff rate of gas is generally several magnitudes higher than that of the liquid. When CO 2 gas is present in the foam, the leakoff coefficient falls in the range between 0 and 1.37015 $ft/\sqrt{min}$ for gas, and between 0.0005 and 0.1056 $ft/\sqrt{min}$ for liquid. Finally, the methodology and results of this study shed light on the mechanistic understanding of the leakoff properties of multiphase systems and could be used to assist the design of foam fracturing for reservoir stimulation.

03 NATURAL GAS↗