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DOE OSTI2025

Predicting Dynamic-to-Static Correction Factor from Petrophysical Data and Chemostratigraphy using Unsupervised Machine Learning

Estimating static mechanical properties of stratigraphic layers is critical for optimizing subsurface engineering applications. To estimate dynamic-to-static correction factor F ds (static-to-dynamic Young’s modulus ratio) across the Caney shale interval in Oklahoma, USA, we integrated triaxial test measurements and petrophysical data, including well logs and X-ray fluorescence (XRF) using unsupervised machine learning (ML). We used a novel workflow that includes principal component analysis (PCA) to reduce data set dimensionality of well logs and XRF data sets—both separately and combined—creating three scenarios, and later applied inverse distance weighting (IDW) to derive F ds profiles for these scenarios. Furthermore, we applied K-means clustering on each scenario to predict depositional facies, and built a stiffness zonation profile through chemostratigraphic analysis of the terrigenous elements to validate the predicted F ds . The predicted F ds profile from each scenario using the PCA-IDW method was compared with the constant F ds approach from our previous study by calculating the root mean square error (RMSE). The combined data sets scenario yielded the lowest RMSE value of 0.113, while the RMSE values for the well logs and XRF scenarios were 0.131 and 0.129, respectively. In addition, the predicted F ds from the XRF scenario well-matched the stiffness zonation from the chemostratigraphic analysis that was built using the optimized K-means clustering of nine clusters for that scenario. These methods and findings offer a valuable tool for refining lithological classification and improving the F ds profile, potentially enhancing drilling and stimulation strategies for subsurface energy engineering applications.

clastic rock↗

DOE OSTI2013

Analysis of Potential Leakage Pathways and Mineralization within Caprocks for Geologic Storage of CO 2

We used a multifaceted approach to investigate the nature of caprocks above, and the interface between, reservoir-quality rocks that might serve as targets for carbon storage. Fieldwork in southeastern Utah examined the regional- to m-scale nature of faults and fractures across the sedimentiological interfaces. We also used microscopic analyses and mechanical modeling to examine the question as to how the contacts between units interact, and how fractures may allow fluids to move from reservoirs to caprock. Regional-scale analyses using ASTER data enabled us to identify location of alteration, which led to site-specific studies of deformation and fluid flow. In the Jurassic Carmel Formation, a seal for the Navajo Sandstone, we evaluated mesoscale variability in fracture density and morphology and variability in elastic moduli in the Jurassic Carmel Formation, a proposed seal to the underlying Navajo Sandstone for CO 2 geosequestration. By combining mechano-stratigraphic outcrop observations with elastic moduli derived from wireline log data, we characterize the variability in fracture pattern and morphology with the observed variability in rock strength within this heterolithic top seal. Outcrop inventories of discontinuities show fracture densities decrease as bed thickness increases and fracture propagation morphology across lithologic interfaces vary with changing interface type. Dynamic elastic moduli, calculated from wireline log data, show that Young’s modulus varies by up to 40 GPa across depositional interfaces, and by an average of 3 GPa across the reservoir/seal interface. We expect that the mesoscale changes in rock strength will affect the distributions of localized stress and thereby influence fracture propagation and fluid flow behavior within the seal. These data provide a means to closely tie outcrop observations to those derived from subsurface data and estimates of subsurface rock strength. We also studied damage zones associated normal faults in the Permian Cedar Mesa Sandstone, southeastern Utah. These faults are characterized by a single slip surfaces and damage zones containing deformation bands, veins, and joints. Field observations include crosscutting relationships, permeability increase, rock strength decrease, and ultraviolet light induced mineral fluorescence within the damage zone. These field observations combined with the interpreted paragenetic sequence from petrographic analysis, suggests a deformation history of reactivation and several mineralization events in an otherwise low-permeability fault. All deformation bands and veins fluoresce under ultraviolet light, suggesting connectivity and a shared mineralization history. Pre-existing deformation features act as loci for younger deformation and mineralization events, this fault and its damage zone illustrate the importance of the fault damage zone to subsurface fluid flow. We model a simplified stress history in order to understand the importance of rock properties and magnitude of tectonic stress on the deformation features within the damage zone. The moderate confining pressures, possible variations in pore pressure, and the porous, fine-grained nature of the Cedar Mesa Sandstone results in a fault damage zone characterized by enhanced permeability, subsurface fluid flow, and mineralization. Structural setting greatly influences fracture spacing and orientation. Three structural settings were examined and include fault proximity, a fold limb of constant dip, and a setting proximal to the syncline hinge. Fracture spacing and dominant fracture orientation vary at each setting and distinctions between regional and local paleo-stress directions can be made. Joints on the fold limb strike normal to the fold axis/bedding and are interpreted to be sub-parallel to the maximum regional paleo-stress direction as there is no fold related strain. Joints proximal to faults and the syncline hinge may have formed under local stress conditions associated with folding and faulting, and in some cases, are perpendicular to the maximum regional paleo-stress direction. Macroscale analyses of the Iron Wash fault, which cuts most of the stratigraphy of the reservoir- seal analogs, reveals that seal bypass occurs along faults with mixed lithologic composition. While portions of the fault may be effective seals, when modeled as a whole the fault zone cannot support a high CO 2 column. We adapted oil-field methods to calculate column heights and sealing capacities. Examination of the burial and tectonic histories of the rocks, coupled with field- and micro-scale studies, allow us to examine the potential for seal failure using basic rock mechanics failure analyses. These studies reveal that the sealing lithologies experienced multiple episodes of deformation that resulted in numerous fractures and small faults. In a stress state based on burial history and overburden loads, we show that most of the seals could fail with normal to slightly excess pore pressures.

58 GEOSCIENCES↗

DOE OSTI2013

Novel dense membrane for hydrogen separation for energy applications

The main objectives of this project are: (1) Characterization of the thermo mechanical properties of the novel dense HTM bulk sample; (2) Development of a correlation among the intrinsic factors (such as grain size and phase distribution), and the extrinsic factors (such as temperature and atmosphere) and the thermo-mechanical properties (such as strengths and stress) to predict the performance of a HTM system (HTM membrane and porous substrate) ; and (3) Evaluation of the stability of the novel HTM membrane and its property correlations after thermal cycling. Based on all results and analysis of the thermo mechanical properties for the HTM cermet bulk samples, several important conclusions were made. The mean σfs at room temperature is approximately 356 MPa for the HTM cermet. The mean σfs value decreases to 284 MPa as the temperature increases to 850?C. The Difference difference in atmosphere, such as air or N2, had an insignificant effect on the flexural strength values at 850?C for the HTM cermet. The HTM cermet samples at room temperature and at 500?C fractured without any significant plastic deformation. Whereas, at 850?C, the HTM cermet samples fractured, preceded by an extensive plastic deformation. It seems that the HTM cermet behaves more like an elastic material such as a nonmetal ceramic at the room temperature, and more like a ductile material at increased temperature (850?C). The exothermic peak during the TG/DTA tests centered at 600?C is most likely associated with both the enthalpy change of transformation from the amorphous phase into crystalline zirconia and the oxidation of Pd phase in HTM cermet in air. The endothermic peak centered at 800?C is associated with the dissociation of PdO to Pd for the HTM cermet sample in both inert N2 environment and air. There is a corresponding weight gain as oxidation occurs for palladium (Pd) phase to form palladium oxide (PdO) and there is a weight loss as the unstable PdO is dissociated back to Pd and oxygen. The normal stress and shear stresses from the Mohr?s circle indicate that the residual stress in the HTM cermet sample is mainly as compressive residual stress in the magnitude of -135 to -155 MP, and with very little shear stress (in the magnitude of 10 MPa). The magnitude of change in the normal stress and the shear stress is insignificant in the HTM after 120 thermal cycles. However, the principle normal stress changes from compressive to tensile residual stress and there is a significant increase in the shear stress after 500 thermal cycles. The calculated value based on the equation and the Mohr?s circle is found to be consistent with the experimental value for the as-received HTM cermet samples. At some rotation (φ) angle, the residual stress was found to be as tensile stress. Most ceramic material is weak in tension, and develops microscopic cracks. With treatment of 120 thermal cycles between 50?850?C, the HTM- sample exhibited thermally-induced cracks on the surface. Visually observable cracks appeared on the surface of HTM cermet with continuous thermal cycling, after 500 thermal cycles. The XRD powder diffraction analysis indicated an increased amount of crystalline PdO crystalline in HTM cermet after 120 and 500 thermal cycles as compare to the as-received samples. The Pd crystalline peaks were found to significantly decrease in peak intensity with thermal cycling. Higher peak intensity for PdO phase was observed with increased number of thermal cycles. A Monoclinic monoclinic zirconia phase was first identified in the as-received HTM as-received sample. However, with thermal cycling treatment of both 120 and 500 thermal cycles, the M-ZrO2 phase is transformed to the tetragonal YSZ, which is consistent with the thermal analysis results by TG/DTA. Correlations of the microstructural and thermo-mechanical properties of both selected reference material and ANL-3e HTM cermet bulk sample are affected mainly by porosity and microstructural features, such as grain size and pore size/distribution. The Young?s Modulus (E-value), especially, is positively proportional to the flexural strength for materials with similar crystallographic structure. For different crystallographic materials, physical properties such as E and density are independent of mechanical properties, such as flexural strength.. Microstructural properties, particularly, grain size and crystallographic structure, and thermodynamic properties are the main factors affecting the mechanical properties at both room and high temperatures. The oxidation and the plasticity of Pd phase mainly affect the mechanical properties of HTM cermet at high temperature or with thermal cycling treatment. Changes in the residual stress and microstructure affect the mechanical properties of HTM when subjected to high temperature or thermal cycling treatment.

08 HYDROGEN↗

DOE OSTI2015

Hypothesis to Explain the Size Effect Observed in APO-BMI Compression Tests

In 2013 compression tests were performed on cylindrical specimens of carbon-microballoon-APOBMI syntactic foam machined to different lengths (0.25, 0.5, and 2.8 inches1) (Kingston, 2013). In 2014 similar tests were performed on glass-microballoon-APO-BMI of different lengths (~0.15”, ~0.32”, and ~0.57”). In all these tests it was observed that, when strains were calculated from the platen displacement (corrected for machine compliance), the apparent Young’s modulus of the material decreased with specimen size, as shown in Table 1. The reason for this size effect was speculated to be a layer of damage on or near the top and bottom machined surfaces of the specimens (Kingston, Schembri, & Siranosian, 2014). This report examines that hypothesis in further detail.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Compression of 1-mm-thick M9763 cellular silicone foam under lateral confinement

M9763 cellular silicone foam disks (1 mm thick, 28.68 mm diameter, 63% nominal porosity) were compressed under lateral confinement using the Instron Electropuls E10000 load frame. Five (5) loadunload cycles up to 65% compressive strain were performed at a test speed of 1.26 mm/min. Stress vs. strain curves were obtained. Additional specimens were compressed without lateral confinement for comparison. The stress vs. strain curve of the confined specimen essentially overlapped that of the unconfined specimen until ~60% strain when it began to increase more rapidly, indicating lock-up (bulk compression) and the onset of lateral expansion of the unconfined specimen. The slope of the stress vs. strain curve was equal to the Young’s modulus of the solid M9787 material comprising the foam at ~50% strain, which is below the expected 63% lock-up strain. The reason for the discrepancy between the two estimates of lock-up strain is not clear.

42 ENGINEERING↗

DOE OSTI2016

Sensitivity analysis of FeCrAl cladding and U3Si2 fuel under accident conditions

The purpose of this milestone report is to highlight the results of sensitivity analyses performed on two accident tol- erant fuel concepts: U3Si2 fuel and FeCrAl cladding. The BISON fuel performance code under development at Idaho National Laboratory was coupled to Sandia National Laboratories’ DAKOTA software to perform the sensitivity analyses. Both Loss of Coolant (LOCA) and Station blackout (SBO) scenarios were analyzed using main effects studies. The results indicate that for FeCrAl cladding the input parameters with greatest influence on the output metrics of interest (fuel centerline temperature and cladding hoop strain) during the LOCA were the isotropic swelling and fuel enrichment. For U3Si2 the important inputs were found to be the intergranular diffusion coefficient, specific heat, and fuel thermal conductivity. For the SBO scenario, Young’s modulus was found to be influential in FeCrAl in addition to the isotropic swelling and fuel enrichment. Contrarily to the LOCA case, the specific heat of U3Si2 was found to have no effect during the SBO. The intergranular diffusion coefficient and fuel thermal conductivity were still found to be of importance. The results of the sensitivity analyses have identified areas where further research is required including fission gas behavior in U3Si2 and irradiation swelling in FeCrAl. Moreover, the results highlight the need to perform the sensitivity analyses on full length fuel rods for SBO scenarios.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Mechanical Behavior of UO 2 at Sub-grain Length Scales: Quantification of Elastic, Plastic and Creep Properties via Microscale Testing

Techniques were developed to measure properties at sub-grain scales using depleted Uranium Oxide (d-UO2) samples heat-treated to obtain different grain sizes and oxygen stoichiometries, through three main tasks: 1) sample processing and characterization, 2) microscale and conventional testing and 3) modeling. Grain size and crystallography were characterized using Scanning Electron Microscopy (SEM), in conjunction with Electron Backscattering Diffraction (EBSD) and Electron Channeling Contrast Imaging (ECCI). Grains were then carefully selected based on their crystallographic orientations to perform ex-situ micromechanical tests with samples machined via Focused Ion Beam (FIB), with emphasis on micro-cantilever bending. These experiments were performed under controlled atmospheres, to insure stoichiometry control, at temperatures up to 700 °C and allowed measurements involving elastic (effective Young’s modulus), plastic (critical resolved shear stresses) and creep (creep strain rates) behavior. Conventional compression experiments were performed simultaneously to compare with the ex-situ measurements and study potential size effects. Modeling was implemented using anisotropic elasticity and inelastic constitutive relations for plasticity and creep based on kinematics and kinetics of dislocation glide that account for the effects of crystal orientation, and stress. The models will be calibrated and validated using the experimental data. This project provided insight on correlations among stoichiometry, crystallography and mechanical behavior in advanced oxide fuels, provided valuable experimental data to validate and calibrate mesoscale fuel performance codes and also a framework to measure sub-grain scale mechanical properties that should be suitable for use with irradiated samples due to small volumes required. The goals and metrics of the ongoing study of thermo-mechanical behavior in depleted uranium dioxide (d-UO 2 ) outlined in this project have been concluded successfully, resulting in: 1) the successful fabrication, processing, and characterization of large-grained samples with various orientations (up to and including single crystals) having stoichiometric and hyper-stoichiometric O/U ratios; 2) formulation, calibration, and validation of a crystal plasticity constitutive model to describe the creep deformation of UO 2 at the sub-grain length scale (single crystal level) at intermediate temperatures; 3) the successful calibration of a crystal plasticity constitutive model to describe the elasto-plastic deformation of microcantilever beams, also at moderate temperatures. Samples were prepared from natural uranium oxide powder of production-quality provided by Areva. The powder was pressed in a die to a pressure of 100 MPa to produce green pellets with no sintering aids, lubricants, or any other additives. The green pellets were then heated up to 1700 °C under ultra-high purity argon atmosphere (~1 ppm O2). The atmosphere was then changed to 79% Argon, 21% O 2 and the temperature was held at 1700 °C for 2 hours to sinter the pellets under oxidative conditions [1] that are known to increase grain growth kinetics in UO 2 [2]. Samples were then cooled down under Ar-4%H2 atmosphere to reduce the samples back to stoichiometric UO 2 . For macro-scale procedures, testing of UO 2 samples with large grains was performed at 1200 °C using a modified load frame capable of applying dead-weight loads to ensure constant stress conditions, while displacement of the sample produced by the applied load was measured with high precision micrometers to obtain strains. Stress steps were used during testing and the strains were monitored to measured creep strain rates under steady state for each level of stress used, so that stress exponents could be obtained. The results of the mechanical testing, along with sample geometry and crystal orientation of the grains in the samples, as well as post-test sample characterization were used to formulate a viscoplastic model to account for steady state (stage II) creep behavior, along with basic assumptions from crystal plasticity and kinematic constraints due to testing fixtures. In the micro-scale, testing of microcantilever beams at temperatures ranging from 25 to 570 °C was performed in-situ with a scanning electron microscope with a special attachment to apply load and measure displacement while the samples were at temperature. The load-displacement curves obtained showed linear behavior before fracture for all temperatures attempted except 570 °C, where clear deviations from non-linearity were observed before fracture. These deviations were consistently observed for all samples tested for a given orientation. A viscoplastic model was used to account for the presence of inelastic strain, along with basic assumptions from crystal plasticity and beam theory. These models were kept as simple as possible, and results from tests performed in a set of samples with a given crystal orientation were used to calibrate the material constants for the model, while results from a different sample set were then used for validation, thus satisfying the conditions of all main tasks within the parameters of this project. Details of these efforts are outlined in this report.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Mechanical Properties of Woven Composites at Ambient Temperature

This report describes the mechanical characterization of six types of woven composites that Sandia National Laboratories are interested in. These six composites have various combinations of two types of fibers (Carbon-IM7 and Glass-S2) and three types of resins (UF-3362, TC275-1, TC350-1). In this work, two sets of experiments were conducted: quasi-static loading with displacement rate of 2 mm/min (1.3x10 ^(-3) in/s) and high rate loading with displacement of 5.08 m/s (200 in/s). Quasi-static experiments were performed at three loading orientations of 0°, 45°, 90° for all the six composites to fully characterize their mechanical properties. The elastic properties Young's modulus and Poisson's ratio, as well as ultimate stress and strain were obtained from the quasi-static experiments. The high strain rate experiments were performed only on glass fiber composites along 0° angle of loading. The high rate experiments were mainly to study how the strain rate affects the ultimate stress of the glass-fiber composites with different resins.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Mechanical Characterization of Woven Composites at Different Temperatures

This work is to characterize the mechanical properties of the selected composites along both on- and off- fiber axes at the ambient loading condition (+25°C), as well as at the cold (-54°C), and high temperatures (+71°C). A series of tensile experiments were conducted at different material orientations of 0°, 22.5°, 45°, 67.5°, 90° to measure the ultimate strength and strain $σ_{f}, ϵ_{f}$, and material engineering constants, including Young's modulus Ε and Poisson's ratio ν. The composite materials in this study were one carbon composite carbon (AS4C/UF3662) and one E-galss (E-glass/UF3662) composite. They both had the same resin of UF 3362, but with different fibers of carbon AS4C and E-glass. The mechanical loading in this study was limited to the quasi-static loading of 2 mm/min (1.3x10 ^(-3) in/s), which was equivalent to 5x10 (-4) strain rate. These experimental data of the mechanical properties of composites at different loading directions and temperatures were summarized and compared. These experimental results provided database for design engineers to optimize structures through ply angle modifications and for analysts to better predict the component performance.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Long Baseline Neutrino Experiment (LBNE) Target Material Radiation Damage from Energetic Protons of the Brookhaven Linear Isotope Production (BLIP) Facility

In search of a low-Z pion production target for the Long Baseline Neutrino Facility (LBNF) of the Deep Underground Neutrino Experiment (DUNE) various grades of graphite were irradiated with 140-180 MeV protons to fluence up to ~6 10 20 cm -2 and irradiation temperatures in the range of 100-200oC. The objective of the irradiation experiment was to assess the radiation induced changes in the graphite onset by its interaction with energetic protons and deduce some measure of performance and survivability under the design conditions of LBNF. A multi-faceted post-irradiation evaluation was conducted to both qualify and quantify the induced material property changes. These studies included dimensional stability and thermal expansion, damage annealing via thermal cycling, high temperature post-irradiation annealing to mimic irradiation at elevated temperatures, stress-strain behavior, oxidation contribution to the postirradiation analysis, potential influence of the argon atmosphere under which irradiation took place, and lattice evolution. Dilatometry-based techniques were coupled with ultrasound-based annealing methodologies as well as DSC and TGA analyses. X-ray diffraction experiments assessed the lattice parameter changes and SEM analyses were used to study the different graphite grade structures. The multi-faceted post-irradiation evaluation, in conjunction with off-beam analyses, revealed some important facts regarding the choice of a graphite grade. Specifically, it was observed that the microstructure of a grade plays an important role in its dimensional stability. X-ray diffraction data indicated variability in basal plane spacing prior to irradiation with POCO d 002 =3.3833 Å, IG-430 d 002 =3.36814 Å and R7650 d 002 =3.37944 Å. Isotropic graphite grades such as POCO and IG-430 are confirmed to undergo microstructural shrinking under irradiation. All four irradiated graphite grades experience irradiation-induced creep leading to increased Young’s modulus with changes as high as 50% that varies with microstructure. X-ray diffraction on irradiated graphite confirmed previously made observations where under both energetic protons as well as fast neutrons of fluence > 5 10 20 cm -2 and at temperatures around 200°C acceleration of the effects on both the micro-and macrostructure is observed. Amongst the irradiated grades POCO graphite showed tendency to increase crystallinity order but also shows turbostratic state resulting from the interaction of its lattice with protons. This report presents and discusses the details of the irradiation experiment and the results of the postirradiation evaluation with main objective the assessment of the applicability and survivability of the selected four graphite grades as high-power accelerators pion production targets where the structural integrity, density reduction, dimensional and physical property stability are of paramount importance.

43 PARTICLE ACCELERATORS↗

DOE OSTI2019

Effects of Electron Irradiation on Candidate Materials for Target Window in Accelerator-Driven Molybdenum-99 Production

NorthStar Medical technologies is planning to produce Mo-99 through the photo-nuclear reaction Mo-100 (γ,n) Mo-99 utilizing multiple high-power electron accelerators. In this approach, the production target consists of multiple thin disks of metal Mo-100 cooled by helium gas at high (300–400 psi) pressure [4]. The cost of enriched Mo-100 is on the order of $500 - 1,000 per gram, which makes a smaller target desirable and requires achieving the highest possible electron flux on the target. The heat deposition in the entrance window limits the maximum flux because the window separates the vacuum in the accelerator beam line from the high-pressure helium in the target and is only cooled on one side by the helium flow. Because the window is continuously under stress from the helium pressure and the heat from the electron beam, it is desirable to estimate a lifetime for the window and develop a replacement schedule for the target holder. Such an estimate requires the ability to predict changes in the window material properties under electron irradiation. Candidate materials for the Mo-99 production target window are Inconel 718, 250 maraging steel, and beryllium. These materials encompass a wide range of thermal conductivity, thermal expansion coefficients, Young’s modulus, tensile strength and tensile ductility. The Mo-99 target window is subjected to internal pressure from the helium coolant and thermal stresses. The operating conditions and relative advantages of each material have been described previously [1]. The current work investigates the effects of electron irradiation on the tensile properties of these materials. Axial tensile tests were conducted with electron-irradiated samples and results were compared to baseline results generated for as-fabricated materials.

36 MATERIALS SCIENCE↗

DOE OSTI2019

In-situ small-scale mechanical testing of fast reactor mixed oxide pins: completion report

The present work represents a pioneering study in the application of advanced techniques to measure micro-mechanical properties of highly radioactive advanced nuclear fuels. First data of Young’s modulus and hardness of fast reactor MOX at burnup exceeding 150 GWd/tHM have been obtained. Despite the challenges encountered in the current work due to equipment malfunction, the experimental approach sought in this work has been proved successful in obtaining new data of high relevance for fuel performance on system with high Pu content and high radiotoxicity with extremely limited exposure to personnel. Further experiments will be conducted in the future based on the present approach, leveraging the experience gained in this project.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2017

Effect of wheel speed on the magnetic and mechanical properties of melt spun Fe-6.5 wt.% electric steel

Fe-Si electric steel is the most widely used soft magnetic materials in electric mahines and motors, transformers and generators. Improving the surperior magnetic and electric properties of 6.5 wt.% high silicon steel is essential for higher may improve energy efficiency and power density of electric machines. However, the brittleness due to the formation of B2 and D03 ordered phases in high silicon steel make it difficult forbids for the application of high silicon steel. It is known that these ordered phases can be fully or partially suppressed by rapid cooling. However, further study is needed to understand the extend of cooling on the magnetic and mechanical properties of 6.5 wt.% silicon steel with various degree of ordering. By tuning the wheel speed from 1m/s to 30m/s with several intervals of the melt spinning process, varying degrees of cooling were achieved on 6.5 wt.% silicon steel ribbons. The cooling rate significant altered the ordering, microstructure size scale, and thus the mechanical and magnetic properties. TEM results showed that D03 ordering can be fully suppressed at high wheel speed, but started to nucleate at 5m/s and below, which correlates with the hardness and Young’s modulus increase towards low wheel speeds as tested by micro and nano indentation. The grain sizes of the ribbons on the wheel side decreased with increasing wheel speeds being ~100 micron at 1m/s and ~8 micron at 30m/s, which led to the change in coercivity. Saturation magnetization and electric resistivity of the ribbons remained about 190 emu/g and 84 microhm *cm, which appeared to be mainly depend on the chemistry.

Fe-6.5%Si Steel↗

DOE OSTI2021

Simulated Adhesive Response to Aging (CRADA 453 Final Report)

The goal of this project was to develop a suite of molecular models to investigate adhesive performance as a result of the presence of different levels of moisture. These different levels of moisture are accepted in the adhesives community to represent different states of aging. First, our team modeled the adhesive’s crosslinked structure. Next, we modeled adding water to the crosslinked structure and used high performance computing resources to simulate water diffusion through the bulk adhesive and possible sites for chain scission. Finally, we modeled the response of the simulated adhesive to tensile loads at various levels of moisture content. These simulations were validated by experimental characterization by the industry partner. We found that the Young’s modulus of the adhesive decreased by about 30% when the water content increased to 3 wt.%. Our simulations also identified the likely site where the polymer chain could break. Our integration of molecular level simulations and mechanical property predictions using high performance computing with experimental studies of a hydrated epoxy system has yielded fundamental insights that will help industry advance lightweight joining technologies.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Ultrasonic Measurements of Temperature Profile and Heat Fluxes in Coal-Fired Power Plants (Final Report)

Many industrial processes are inaccessible or inhospitable to characterization by traditional temperature measurement methods, such as thermocouples, especially over prolonged exposure to harsh environments. Ultrasound is an established characterization technology with diverse applications ranging from medical imaging to therapies to flaw detection to nondestructive evaluation. Ultrasound may characterize solid materials and components noninvasively as a nondestructive evaluation modality and obtain internal measurements of material properties. For example, the speed of ultrasound propagation changes with Young’s modulus and Poisson’s ratio, which can be found from its measurements. Traditional ultrasonic characterization assumes all material properties remain constant with the position. When this assumption holds, a property of interest may be measured by relating it to the speed of ultrasound propagation (or a speed of sound, SOS) and measuring the SOS by timing the ultrasound propagation through a known distance. However, when a property of interest is spatially distributed, the propagation time depends on the SOS changing with the position along the ultrasound propagation path. The multiple temperature distributions may lead to an identical time of flight (TOF). Temperature is one property that impacts the speed of ultrasound and often cannot be assumed to remain constant with the position. Previously, in the context of temperature, we addressed the challenge of ultrasonic characterization of spatially distributed properties by developing a method for measuring segmental temperature distributions (MSTD). This method divides the ultrasonic propagation into segments bound by echogenic features. These features provide ultrasonic interfaces where some energy is reflected toward the receiving transducer, and the rest continues through the medium. The time-of-flight between the echoes reflected from echogenic features characterizes the spatial distribution in the properties of interest in the corresponding segment of the ultrasonic propagation path. This project demonstrated the application of the MSTD method in industrial conditions of the coal-fired power plant. We implemented the MSTD using metals and alloys waveguides, which may be the existing structure for which the temperature distribution is characterized or purposefully designed waveguides added to the structure by welding or other means specifically to quantify thermal properties using the MSTD method. Previous iterations of the MSTD method used ceramic and cementitious waveguides, which significantly attenuate ultrasound. On the other hand, low attenuation in metallic waveguides creates interactions between echogenic features which compilates the signal analysis in the segmental TOF measurements. We have established the WG design principles that minimize the interferences between trailing and primary echoes and, in some cases, eliminate them. The waveguides in which echoes do not interfere improve the timing accuracy and the robustness of ultrasonic measurements of the spatial distributions in material properties. Our emphasis remained on the estimation of the temperature distributions. We have developed general recommendations for designing ultrasonically segmented waveguides with the reduced influence of trailing echoes. Two of our waveguide designs were tested in the industry. The first waveguide was designed for insertion into a combustion zone of the utility-scale coal-fired power plant boiler. The second design allows the characterization of temperature distribution in the direction normal to the boiler’s water wall, a large heat exchanger converting the chemical energy released during combustion to the steam driving the electrical power generation turbines. These waveguides were designed to operate within a restrictive space of thermally insulated water wall and incorporate densely located echogenic features while combatting the influence of trailing echoes. The project has successfully demonstrated the feasibility of using the developed method for accurate, continuous, and robust temperature measurements in extreme environments of power generation and other industrial processes. It, therefore, has achieved its overarching goal of advancing the technology readiness level of the novel Ultrasound Measurements of Segmental Temperature Distribution (US-MSTD) method for real-time measurements of the temperature distribution and heat fluxes closer to commercial availability, developing a prototype multipoint measurement system, and validating its performance on coal-fired utility boilers. The success of this project was achieved in collaboration with the power generator, Rocky Mountain Power, and set the stage for the transfer of this technology from the laboratory to the industry.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2022

Microbial Curing of Cement for Energy Applications

Rutgers University, Lawrence Livermore National Laboratory, and the University of Arizona executed this program over 36 months with a 4-Task Program: (M1)-Microbial Engineering (M2)-Microstructure Modelling, (M3) Cement and Concrete Formulation, (M4)-Techno-economic analysis (TEA) and lifecycle assessment (LCA). This program developed a new carbonate cement concrete manufacturing process called microbial curing (MBC). MBC utilizes in-situ microbial production of CO 2 that dissolves into pore-bound water to carbonate a cementitious material creating a bonding matrix of CaCO 3 and SiO 2 that hardens and densifies the material. This is the first work of this type where calcium silicate was used in microbial studies. All other work reported in the literature always used a soluble form of calcium. This final report describes the work done in the final quarter, the best procedures and results, and the final techno-economic and lifecycle analyses. This quarter, we cast and cured twenty-five (4”x8”) cylinder samples. The compressive strength, split tensile, Young’s modulus, chloride permeability, and creep measurements were performed. These measurements demonstrated that MBC of calcium silicate concrete exhibits scaling problems due to the escape of ammonia gas, a product of the microbial reaction to generate CO 2 . As curing proceeds, the ability for the gas to escape from within the cylinder is restricted by the outer cylindrical portions densifying, making the outer portion highly impermeable to gas flow. In contrast, the small samples cured are uniformly cured, forming materials whose mechanical properties are 7x better than the large samples. This problem needs to be solved before this technology can be commercialized. The techno-economic and lifecycle analyses indicate that the technology developed in this program exhibits a significant opportunity to reduce the cost of cement and CO 2 emissions associated with concrete, provided the curing issue associated with larger samples can be addressed.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Interpreting the Strain Tensor During Injection into a Reservoir

A suite of well tests was conducted to evaluate the feasibility of measuring and interpreting the strain tensor during injection. Water was injected at 1 liter/s for a few days to a few weeks into a well completed at a depth of 530 m in the Bartlesville sandstone in the North Avant Field in Oklahoma. The strain tensor was measured using strainmeters at a depth of 30m and a distance of 220m from the well. We used a Gladwin strainmeter, a state-of-the-art geodetic strainmeter, as well as novel borehole strainmeters developed for the project. After processing, the horizontal strains were tensile and the vertical strain was compressive during injection. The radial strain was less than the circumferential strain. Strain magnitudes increased during injection and recovered afterward. The strain rate was as fast as 100 nanostrain/d at the start of injection, and decreased to 10 nanostrain/d after a few days. The normal strain signals were approximately proportional to the log of time during the first few days of injection, and the semi-log slope was 50 to 75 nanostrain. Data from the Gladwin strainmeter were essentially identical to data from a strainmeter we developed using optical fiber sensors. Tilt was measured using two tiltmeters, but the tilts were erratic compared to the normal strain and were of limited value. Strain data were analyzed using a strain type-curve method, an analytical solution to a poroelastic inhomogeneity, and a stochastic inversion method. Poroelastic simulations explain the data well. Results from the interpretation methods are consistent with each other, and with independent information characterizing the area. The hydraulic diffusivity is approximately 0.5 m2/s and the permeability is between 100 and 500 mD, according to analysis of the strain signals. This is consistent with measurements of permeability from cores, and with analyses of pressure transients. The analyses indicate that Young’s modulus of the reservoir is between 2 and 6 GPa. Strain interpretations indicate the well intersects a permeable lens with a maximum dimension of 500 to 1,000 m. An isopach map of coarse-grained sand confirms a feature roughly 1,000 m in lateral extent. The results demonstrate that the strain signal measured at shallow (30m) depth can be used to infer properties and heterogeneities in an underlying reservoir or aquifer.

Murdoch, Larry↗

DOE OSTI2019

Framework for Characterizing Strain in the Vicinity of Leaky Reservoirs

The identification of leaks in the vicinity of reservoirs is critical to determining the feasibility of long-term geologic storage of CO2, methane, wastewater and other fluids. We have established a series of basic reservoir leakage scenarios and performed numerical analysis to characterize the associated pressure and strain fields created from injection into these leaky reservoir settings, as well from ambient loads, such as barometric pressure and earth tides. The end-member conceptual models evaluated include injection and ambient loads applied to: 1) a thin, horizontal layer with no leakage pathways (baseline), 2) a thin layer with a vertical conduit to the surface (e.g., a leaky fault or abandoned well) and 3) a thin layer with a conduit to an overlying aquifer. The pressure and strain fields are sensitive to the reservoir and confining unit geometry, material properties, the distribution, composition and compressibility of the pore fluid and the type of applied load (e.g., constant vs. cyclical injection, barometric pressure fluctuations, earth tides, etc.). Initial results from the numerical analyses indicate that an induced pressure change of 1 MPa in a formation at 1 km depth with a Young’s modulus of 10 GPa is sufficient to create vertical and horizontal strain signals as high as 2 με at a depth of 100 m. The signals predicted from leaky conditions compared to an intact reservoir differ by as much as 0.2 με in magnitude and evolve at different rates. We have developed instruments capable of measuring vertical and horizontal strain at a resolution of better than 5 nε and have recorded repeatable strain signals at 30 m depth in response to wastewater injection into the Avant field in Oklahoma. Based on these findings, strain signals predicted in the shallow subsurface (< 100 m) with numerical analysis are expected to be measurable, and this signal may be inverted to characterize the location and magnitude of leaks, as well as to characterize the geometry and hydromechanical properties of the formation and overlying confining units. This suggests that shallow strain measurements could be a cost effective method for characterizing and monitoring gas storage projects.

Robert, Moak↗