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NASA NTRS1984

The effect of space environment exposure on the properties of polymer matrix composite materials (A0180)

The objective of this experiment is to determine the effect of various lengths of exposure to a space environment on the mechanical properties of selected commercial polymer matrix composite materials. Fiber materials will include graphite, boron, S-glass, and PRD-49. The mechanical properties to be investigated are orthotropic elastic constants, strength parameters (satisfying the tensor polynomial relation), coefficients of thermal expansion, impact resistance, crack propagation, and fracture toughness. In addition, the effect of laminate thickness on property changes will also be investigated.

Tennyson, R. C.↗

DOE OSTI2023

Tunable thermoplastic elastomer gels derived from controlled-distribution triblock copolymers with crystallizable endblocks

Thermoplastic elastomers (TPEs), a commercially important category of triblock copolymers, are employed alone or upon physical modification with a midblock-selective oil (to form TPE gels, TPEGs) in a broad range of contemporary technologies. While most copolymers in this class of self-networking macromolecules possess glassy polystyrene endblocks and a rubbery polydiene or polyolefin midblock, we investigate TPEGs fabricated from a novel controlled-distribution copolymer with crystallizable polyolefin endblocks and a random-copolymer midblock. According to both electron microscopy and small-angle scattering, the morphologies of these TPEGs remain largely invariant up to 40 wt% oil and then transform considerably at higher oil levels. Although reductions in endblock melting point and crystallinity measured by thermal calorimetry accompany increasing oil content, mechanical properties such as the uniaxial strain at break and fracture toughness improve in some cases by over 50% between 5 and 40 wt% oil. In fact, the strain at break can reach 2500% within this range, thereby confirming that (i) the structure–property relationships of these unique TPEGs are highly composition-tunable and (ii) these TPEGs, stabilized by crystallizable endblocks, provide an attractive alternative for ultrasoft and stretchy recyclable materials.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Influence of injection-induced cooling on deviatoric stress and shear reactivation of preexisting fractures in Enhanced Geothermal Systems

Cold water injection into a hot, fractured, geothermal reservoir may trigger shear activation of pre-existing fractures that can help to enhance reservoir permeability, but may also result in unwanted seismicity. In this study, we investigate through numerical modeling of a hypothetical geothermal reservoir how injection-induced cooling may influence the potential for shear activation, paying special attention to the evolution of deviatoric stress under various stress regimes. In each case, we consider either a reservoir with homogeneous hydraulic properties or the presence of a more permeable fracture zone intersecting the injection well. This fracture zone is either oriented in the maximum (S Hmax ) or minimum (S hmin ) horizontal stress direction. Finally, our main finding is that depending on the configuration, injection-induced cooling stresses can favor or prevent shear reactivation of the preexisting fracture, and this effect can vary temporally and spatially.

58 GEOSCIENCES↗

DOE OSTI2021

Multiscale Modeling of Cr 2 O 3 -doped UO 2 Creep and Fracture

The pursuit of UO 2 fuel with various dopants (e.g., Cr 2 O 3 , Al 2 O 3 ) for improved accident tolerance due to larger grain sizes and suspected reductions in fission gas release and creep requires advanced modeling and simulation tools. These tools enable rapid multiscale development and understanding of material behavior in regimes where experimental measurements may be lacking. This work builds upon previous multiscale modeling efforts for fission gas behavior of Cr 2 O 3 -doped UO 2 to begin looking at the effects of dopants on mechanical properties with a particular focus on creep and fracture. The results indicate that dislocation climb is the most dominate creep mechanism at almost all temperatures with sensitivity analyses further providing evidence in support of that claim. Limited experimental data from the Advanced Fuels Campaign (AFC) program in the U. S. Department of Energy on tensile strength of Cr 2 O 3 -doped UO 2 indicates that fracture may be less severe in doped specimens. The results on creep and fracture are preliminary given the large uncertainty associated with the models.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Surfactants are Ineffective for Reducing Imbibition of Water-Based Fracturing Fluids in Deep Gas Reservoirs

Minimizing loss of injected hydraulic fracturing fluids into shale along fracture-matrix boundaries is desired because imbibed water restricts gas production and wastes valuable water resources. This problem has motivated the addition of surfactants into water-based hydraulic fracturing fluids in order to reduce the capillary driving force for imbibition. Here, we show that reduction in interfacial tension and wettability alteration has negligible ability to reduce imbibition in deep gas reservoirs. The effectiveness of altering capillary forces acting at the wetting front also depends on the injection pressure acting at the fracture-matrix boundary. The pressure at the interface between the fracture and the shale matrix is constrained between the reservoir pore pressure and formation pressure (rock fracture pressure, also known as breakdown pressure of the rock) and increases with depth to magnitudes that greatly exceed that of capillary pressures. Furthermore, the analyses presented here show that even maximum alteration of interfacial properties that result in strongly hydrophobic interactions between the fracturing fluid and reservoir rock is incapable of significantly reducing imbibition in deep reservoirs. Instead of using surfactants, this analysis points to decreases in wellbore shut-in pressures and shut-in times as practical options for reducing imbibition losses of water-based fluids.

03 NATURAL GAS↗

DOE OSTI2022

Multiscale Modeling of Cr 2 O 3 -doped UO 2 Creep and Fracture (Rev.1)

The pursuit of UO 2 fuel with various dopants (e.g., Cr 2 O 3 and Al 2 O 3 ) for improved accident tolerance due to larger grain sizes and suspected reductions in fission gas release and creep requires advanced modeling and simulation tools. Such tools enable rapid multiscale development and enhanced understanding of material behavior in regimes for which experimental measurements may be lacking. This work builds on previous multiscale modeling efforts targeting the fission gas behavior of Cr 2 O 3 -doped UO 2 , in order to begin exploring the effects of dopants on mechanical properties, with a particular focus on creep and fracture. The results indicate that dislocation climb is the most dominate creep mechanism at almost all temperatures, and sensitivity analyses provide evidence in further support of this claim. The limited experimental data generated by the U.S. Department of Energy’s Advanced Fuels Campaign (AFC) on the tensile strength of Cr 2 O 3 -doped UO 2 indicate that fracture may be less severe in doped specimens. The results on creep and fracture are preliminary, given the large degree of uncertainty associated with the models.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

A Critical Review of the Physicochemical Impacts of Water Chemistry on Shale in Hydraulic Fracturing Systems

Hydraulic fracturing of unconventional hydrocarbon resources involves the sequential injection of a high-pressure, particle-laden fluid with varying pH’s to make commercial production viable in low permeability rocks. This process both requires and produces extraordinary volumes of water. The water used for hydraulic fracturing is typically fresh, whereas “flowback” water is typically saline with a variety of additives which complicate safe disposal. As production operations continue to expand, there is an increasing interest in treating and reusing this high-salinity produced water for further fracturing. Here in this paper we review the relevant transport and geochemical properties of shales, and critically analyze the impact of water chemistry (including produced water) on these properties. We discuss five major geochemical mechanisms that are prominently involved in the temporal and spatial evolution of fractures during the stimulation and production phase: shale softening, mineral dissolution, mineral precipitation, fines migration, and wettability alteration. A higher salinity fluid creates both benefits and complications in controlling these mechanisms. For example, higher salinity fluid inhibits clay dispersion, but simultaneously requires more additives to achieve appropriate viscosity for proppant emplacement. In total this review highlights the nuances of enhanced hydrogeochemical shale stimulation in relation to the choice of fracturing fluid chemistry.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1996

Development and Processing of Nickel Aluminide-Carbide Alloys

With the upper temperature limit of the Ni-based superalloys attained, a new class of materials is required. Intermetallics appear as likely candidates because of their attractive physical properties. With a relatively low density, high thermal conductivity, excellent oxidation resistance, high melting point, and simple crystal structure, nickel aluminide (NiAl) appears to be a potential candidate. However, NiAl is limited in structural applications due to its low room temperature fracture toughness and poor elevated temperature strength. One approach to improving these properties has been through the application of eutectic composites. Researchers have shown that containerless directional solidification of NiAl-based eutectic alloys can provide improvement in both the creep strength and fracture toughness. Although these systems have shown improvements in the mechanical properties, the presence of refractory metals increases the density significantly in some alloys. Lower density systems, such as the carbides, nitrides, and borides, may provide NiAl-based eutectic structure. With little or no information available on these systems, experimental investigation is required. The objective of this research was to locate and develop NiAl-carbide eutectic alloys. Exploratory arc-melts were performed in NiAl-refractory metal-C systems. Refractory metal systems investigated included Co, Cr, Fe, Hf, Mo, Nb, Ta, Ti, W, and Zr. Systems containing carbides with excellent stability (i.e.,HfC, NbC, TaC, TiC, and ZrC) produced large blocky cubic carbides in an NiAl matrix. The carbides appeared to have formed in the liquid state and were randomly distributed throughout the polycrystalline NiAl. The Co, Cr, Fe, Mo, and W systems contained NiAl dendrites with a two-phase interdendritic microconstituent present. Of these systems, the NiAl-Mo-C system had the most promising microstructure for in-situ composites. Three processing techniques were used to evaluate the NiAl-Mo-C system: arc-melting, slow cooling, and containerless directional solidification. Arc-melting provided a wide range of compositions in an economical and simple fashion. The slow cooled ingots provided larger ingots and slower cooling rates than arc-melting. Directional solidification was used to produce in-situ composites consisting of NiAl reinforced with molybdenum carbides.

Newport, Timothy Scott↗

DOE OSTI2017

High Damping of Lightweight TiNi-Ti{sub 2}Ni Shape Memory Composites for Wide Temperature Range Usage

A bimodal porous TiNi-Ti{sub 2}Ni shape memory alloy composite (SMAC) with 59% porosity was fabricated by sintering Ti-46at.%Ni elemental powders with pore-forming agent. The porous TiNi-Ti{sub 2}Ni SMAC contains two irregular pores of about 400 and 120 μm. We investigated the microstructure and pore morphology correlated with the mechanical properties and damping capacities of the SMAC. Ti{sub 2}Ni intermetallic phases with size of 1-3 μm were homogeneously distributed in the TiNi matrix. The porous TiNi-Ti{sub 2}Ni SMAC exhibits exceptionally high inverse mechanical quality factor (Q{sup −1}) of ~0.25 at < 40 °C, which is among the highest value reported for porous/dense shape memory alloys or composites to best of our knowledge, and it shows very high compressive fracture strain of about 25%. Moreover, the fabricated porous SMAC at relatively low strain amplitude can exhibit considerable high Q{sup −1} of 0.06 ~ 0.11 for a wide range of temperature between − 90 and 200 °C, which is attributed to the stress concentration distribution provided by the bimodal structure of pores and the massive interfaces between pore/matrix and TiNi/Ti{sub 2}Ni. These porous SMACs can be an ideal candidate for using as a lightweight damping material in the energy-saving applications.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Fracture Toughness of High-Cr Steels after Various Thermomechanical Treatments

This research aimed to improve the mechanical properties of high-Cr steels by developing new thermomechanical processes for application to advanced fast reactors. A simultaneous improvement of fracture toughness and strength was specifically targeted in the design of thermomechanical processing for various 9Cr and 12Cr steels. For the structural materials of fusion and fast reactors, the high-chromium steels with fine ferritic/martensitic (FM) structures are favored because of their high creep strength and excellent resistance to high-temperature radiation damage such as void swelling. After the traditional thermomechanical treatment consisting of normalizing, water quenching, and tempering, however, the high-Cr steels show limited mechanical properties at high temperatures, e.g., significant decrease of strength above ~450°C. Since the high-Cr steels are tempered at high temperatures (typically around 750°C), significant coarsening of the lath structure and carbides and annihilation of dislocations occur in the final thermomechanical treatment. It is believed that the high-temperature tempering can maximize the ductility of the FM steels, but their high-temperature strength is reduced and often with high-temperature fracture toughness. It is also likely that such a fully-tempered structure will demonstrate a lowered radiation resistance when compared to the steels with finer structures. This research was planned to explore new processing routes that can produce ultrafine microstructures and thus can improve the high-temperature mechanical properties of the high-Cr steels. In this research, three 9Cr steels and two 12Cr steels were selected and a series of new thermomechanical process treatments (TMTs) were designed and applied to the five steels to find the TMT routes that will result in increase of both strength and fracture toughness. It was demonstrated for HT-9 steels that some tailored TMTs increased or maintained the fracture toughness of the high-Cr steels while the treatments could significantly increase their strength to the level comparable to those of nanostructured ferritic alloys. This report compares the fracture toughness data of both 9Cr and 12Cr steels after various thermomechanical treatments with the reference data of similar steels. A two-step tempering route is selected for application to the high-Cr steels for reactor core structures.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Fully coupled hydro-mechanical numerical manifold modeling of porous rock with dominant fractures

Coupled hydro-mechanical (HM) processes are significant in geological engineering such as oil and gas extraction, geothermal energy, nuclear waste disposal and for the safety assessment of dam foundations and rock slopes, where the geological media usually consist of fractured rock masses. We developed a model for the analysis of coupled hydro-mechanical processes in porous rock containing dominant fractures, by using the numerical manifold method (NMM). In the current model, the fractures are regarded as different material domains from surrounding rock, i.e., finite-thickness fracture zones as porous media. Compared with the rock matrix, these fractured porous media are characterized with nonlinear behavior of hydraulic and mechanical properties, involving not only direct (poroelastic) coupling but also indirect (property change) coupling. By combining the potential energy associated with mechanical responses, fluid flow and solid–fluid interactions, a new formulation for direct HM coupling in porous media is established. For indirect coupling associated with fracture opening/closure, we developed a new approach implicitly considering the nonlinear properties by directly assembling the corresponding strain energy. Compared with traditional methods with approximation of the nonlinear constitutive equations, this new formulation achieves a more accurate representation of the nonlinear behavior. We implemented the new model for coupled HM analysis in NMM, which has fixed mathematical grid and accurate integration, and developed a new computer code. We tested the code for direct coupling on two classical poroelastic problems with coarse mesh and compared the results with the analytical solutions, achieving excellent agreement, respectively. We tested for indirect coupling on models with a single dominant fracture and obtained reasonable results. The current poroelastic NNM model with a continuous finite-thickness fracture zone will be further developed considering thin fractures in a discontinuous approach for a comprehensive model for HM analysis in fractured porous rock masses.

58 GEOSCIENCES↗

NASA NTRS2015

Characterization of Machine Variability and Progressive Heat Treatment in Selective Laser Melting of Inconel 718

The absence of an economy of scale in spaceflight hardware makes additive manufacturing an immensely attractive option for propulsion components. As additive manufacturing techniques are increasingly adopted by government and industry to produce propulsion hardware in human-rated systems, significant development efforts are needed to establish these methods as reliable alternatives to conventional subtractive manufacturing. One of the critical challenges facing powder bed fusion techniques in this application is variability between machines used to perform builds. Even with implementation of robust process controls, it is possible for two machines operating at identical parameters with equivalent base materials to produce specimens with slightly different material properties. The machine variability study presented here evaluates 60 specimens of identical geometry built using the same parameters. 30 samples were produced on machine 1 (M1) and the other 30 samples were built on machine 2 (M2). Each of the 30-sample sets were further subdivided into three subsets (with 10 specimens in each subset) to assess the effect of progressive heat treatment on machine variability. The three categories for post-processing were: stress relief, stress relief followed by hot isostatic press (HIP), and stress relief followed by HIP followed by heat treatment per AMS 5664. Each specimen (a round, smooth tensile) was mechanically tested per ASTM E8. Two formal statistical techniques, hypothesis testing for equivalency of means and one-way analysis of variance (ANOVA), were applied to characterize the impact of machine variability and heat treatment on six material properties: tensile stress, yield stress, modulus of elasticity, fracture elongation, and reduction of area. This work represents the type of development effort that is critical as NASA, academia, and the industrial base work collaboratively to establish a path to certification for additively manufactured parts. For future flight programs, NASA and its commercial partners will procure parts from vendors who will use a diverse range of machines to produce parts and, as such, it is essential that the AM community develop a sound understanding of the degree to which machine variability impacts material properties.

Prater, T.↗

NASA NTRS2015

Characterization of Machine Variability and Progressive Heat Treatment in Selective Laser Melting of Inconel 718

The absence of an economy of scale in spaceflight hardware makes additive manufacturing an immensely attractive option for propulsion components. As additive manufacturing techniques are increasingly adopted by government and industry to produce propulsion hardware in human‐rated systems, significant development efforts are needed to establish these methods as reliable alternatives to conventional subtractive manufacturing. One of the critical challenges facing powder bed fusion techniques in this application is variability between machines used to perform builds. Even with implementation of robust process controls, it is possible for two machines operating at identical parameters with equivalent base materials to produce specimens with slightly different material properties. The machine variability study presented here evaluates 60 specimens of identical geometry built using the same parameters. 30 samples were produced on machine 1 (M1) and the other 30 samples were built on machine 2 (M2). Each of the 30‐sample sets were further subdivided into three subsets (with 10 specimens in each subset) to assess the effect of progressive heat treatment on machine variability. The three categories for post‐processing were: stress relief, stress relief followed by hot isostatic press (HIP), and stress relief followed by HIP followed by heat treatment per AMS 5664. Each specimen (a round, smooth tensile) was mechanically tested per ASTM E8. Two formal statistical techniques, hypothesis testing for equivalency of means and one‐way analysis of variance (ANOVA), were applied to characterize the impact of machine variability and heat treatment on six material properties: tensile stress, yield stress, modulus of elasticity, fracture elongation, and reduction of area. This work represents the type of development effort that is critical as NASA, academia, and the industrial base work collaboratively to establish a path to certification for additively manufactured parts. For future flight programs, NASA and its commercial partners will procure parts from vendors who will use a diverse range of machines to produce parts and, as such, it is essential that the AM community develop a sound understanding of the degree to which machine variability impacts material properties.

Prater, Tracie↗

DOE OSTI2021

Stress-sensitivity of fracture conductivity of Tuscaloosa Marine Shale cores

Production decline from wells producing from shale rocks is typically quite rapid. One possible factor responsible for such decline is loss in fracture conductivity. This is true in the case of the Tuscaloosa Marine shale reservoir. In this work, the stress-dependent fracture conductivity of TMS core samples is investigated using five propped cores under varying stress conditions. In addition, the effects of static rock mechanical properties and rock mineralogy on conductivity decline are investigated. The mineralogy of each core sample was determined by X-ray Diffraction analysis. Fracture conductivity was measured using a Hassler-type pressure core holder with a pressure rating of 15,000 psi (103.42 MPa). Estimated rock mechanical properties showed that shale anisotropy could affect fracture conductivity. The time decline in conductivity revealed two possible decline trends, a) decline from the reduction in induced fracture width, and b) decline from the healing of developed micro-cracks. An exponential decline in fracture conductivity with increasing confinement pressure was observed with an average decline rate constant of 3.15 x 10 -10 mPa -1 . While rock mineralogy did not have any clear relationship with conductivity decline, the effects of rock mechanical properties were only important at 10.34 MPa confinement pressure and above. The observation showed that a high Young's modulus correlate to high conductivity, whereas a high Poisson's ratio correlate to low conductivity. This study provides useful observations for optimizing fracture design to enhance well productivity in the TMS.

02 PETROLEUM↗

NASA NTRS1990

Composite structure global fracture toughness via computational simulation

A computational method for the simulation of damage and fracture propagation in laminated composites is presented. A quantitative evaluation of the global fracture toughness of composites is shown as a tool for monitoring the fracture stability of composites under sustained loading. Changes in overall structural properties such as natural frequencies and the fundamental buckling load are also computed with increasing load-induced damage. Structural degradation, delamination, fracture, and damage propagation are included in the simulation. An angle-plied composite plate structure subjected to inplane tensile loading is used as an example to demonstrate some of the feature of the computational method.

Minnetyan, L.↗

DOE OSTI2023

Atomistic simulation of brittle-to-ductile transition in silicon carbide embedded with nano-sized helium bubbles

In this study, the tensile response of cubic silicon carbide (SiC) bulk containing cavities (voids and He bubbles) has been investigated using molecular dynamic simulations. The formation of cavities in SiC leads to a significant degradation in the mechanical properties of SiC with more influence on material fracture than initial elastic deformation. The brittle-to-ductile transition occurs in cavity-embedded SiC as the pressure in He bubbles increases. This is associated with the deformation mechanism that bond breaking at a low He bubble pressure transfers to extensive dislocation activities at a higher He bubble pressure. The cavities can effectively concentrate stress around them in the direction perpendicular to the tension, which leads to preferred cracking in the region with a higher tensile stress. The failure mechanism as revealed by this study improves understanding of property degradation in SiC that may be useful for applications of SiC in advanced nuclear energy systems.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

NASA NTRS1977

Friction, deformation and fracture of single-crystal silicon carbide

An investigation was conducted to determine the nature of the deformation and fracture of silicon carbide and its effects on friction properties. Friction experiments were conducted with hemispherical and conical diamond riders sliding on the basal plane of silicon carbide. The results indicate that, when deformation is primarily elastic, the friction does not depend on crystallographic orientation and there is no detectable fracture or cracking. When, however, plastic deformation occurs, silicon carbide exhibits anisotropic friction and deformation behavior. Surface fracture crack patterns surrounding wear tracks are observed to be of three types. The crack-geometries of two types are generally independent of orientation, the third crack, however, depends on the orientation. All surface cracks extend into subsurface.

Miyoshi, K.↗

DOE OSTI2021

Multiscale Characterization of the Caney Shale — An Emerging Play in Oklahoma

From a hydrocarbon perspective, the Caney Shale has historically been evaluated as a sealing unit, which resulted in limited studies characterizing the rock properties of the Caney Shale and its suitability for hydraulic fracturing. The objective of our research is to help bridge the current knowledge gap through the integration of multiscale laboratory techniques and to characterize the macro- and microscale rock properties of the Caney Shale. We employed an integrated approach for the characterization of the Caney using 200 ft (61 m) of Caney core from a target well in southern Oklahoma. Core observation and petrographic analysis of thin sections were combined to characterize the general rock types and associated fabrics and textures. Mineralogical composition, pore system architecture, and rock fabric were analyzed using x-ray diffraction (XRD), scanning electron microscopy/energy dispersive x-ray spectroscopy (SEM/EDS), and focused ion beam (FIB)-SEM. In addition, rebound hardness and indentation testing were carried out to determine rock hardness (brittleness) and elasticity, respectively. With the integrated multiscale characterization, three mixed carbonate-siliciclastic rock types were identified — mudstone, calcareous siltstone, and silty carbonate — likely representing a spectrum of deposition from low to relatively high energy environments in the distal portions of a ramp system. Silty carbonate contains mostly interparticle pores. The calcareous siltstones and silty mudstones contain a combination of organic matter pores and interparticle pores. Each of the rock types shows unique mineralogical compositions based on XRD. The mudstone lithofacies has the highest clay content and the least carbonate content. Calcareous siltstones show moderate carbonate and clay content. Silty carbonate indicates the highest carbonate content with the least clay content. In an order of mudstone, calcareous siltstone, and silty carbonate, rebound hardness and Young’s modulus show an increasing trend. As a result of rock-fluid interactions, there are potential scaling reactions during completion and production that could ultimately affect permeability and production rates. Overall, the proposed multiscale integration approach is critical for the geologic characterization of most rocks. However, in shale reservoirs dominated by microporosity and microstructure where engineered fractures are expected to provide permeability at a reservoir scale, successful integration is essential. An optimized, integrated geological characterization of the Caney Shale that is well aligned with the engineering designs in drilling, completing, and producing wellbores will ultimately lead to optimal production while providing safe and environmentally responsible operations.

Wang, Yulun↗