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DOE OSTI2023

Testing Various Cement Formulations under Temperature Cycles and Drying Shrinkage for Low-Temperature Geothermal Wells

Low-enthalpy geothermal wells are considered a sustainable energy source, particularly for district heating in the Netherlands. The cement sheath in these wells experiences thermal cycles. The stability of cement recipes under such conditions is not well understood. In this work, thermal cycling experiments for intermediate- and low-temperature geothermal well cements have been conducted. The samples were cured either under ambient conditions or under realistic pressure and temperature for 7 days. The samples did not show any signs of failure after performing 10 cycles of thermal treatment between 100 °C and 18 °C. We also tested cement formulations under drying conditions. Drying shrinkage is caused by a reduction in the water content of cement, which leads to capillary forces that can damage cement. Such circumstances lead to tensile stresses causing radial cracks. Most samples exhibited cracks under low humidity conditions (drying). Fiber reinforcement, especially using short PP fibers, improved the cement’s resilience to temperature and humidity changes. Such additives can improve the longevity of cement sheaths in geothermal wells.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Dynamic Deformation in Nuclear Graphite and Underlying Mechanisms

Time-dependent deformation in nuclear graphite is influenced by the creation and migration of radiation-induced defects in the reactor environment. This study investigates the role of pre-existing defects such as point defect clusters and Mrozowski cracks in nuclear graphite IG-110. Separate specimens were irradiated with a 2.8 MeV Au 2+ beam with a fluence of 4.38 × 10 14 cm −2 and an 8 MeV C 2+ beam with a fluence of 1.24 × 10 16 cm −2 . Microscopic specimens were either mechanically loaded inside a transmission electron microscope (TEM) or subjected to ex situ indentation-based creep loading. In situ TEM tests showed significant plasticity in regions highly localized around the Mrozowski cracks, resembling slip or ripplocation bands. Slip bands were also seen near regions without pre-existing defects but at very high stresses. Ex situ self-ion irradiation embrittled the specimens and decreased the creep displacement and rate, while heavy ion irradiation resulted in the opposite behavior. We hypothesize that the large-sized gold ions (compared to the carbon atoms) induced interplanar swelling as well as cross-plane channels for increased defect mobility. These findings illustrate the role of pre-existing defects in the dynamic relaxation of stresses during irradiation and the need for more studies into the radiation environment’s impact on the mechanical response of nuclear graphite.

creep deformation↗

DOE OSTI2022

Development of Lightweight Structural Materials with Improved Properties for Fission Batteries

Fission batteries require lightweight structural materials that demonstrate structural resilience when subjected to repeated shutdown, transportation, startup cycles, and certain external conditions, including rare events such as seismic vibrations and tsunamis. The objectives of this project are (1) to produce lightweight structural materials whose strength-to-weight ratios and fatigue resistance exceed those of current widely used structural materials such as 316 stainless steels (SS316), and (2) to enhance radiation tolerance of structural materials over a suitable service temperature range. To achieve these, (1) a lattice structure will be produced, (2) advanced modeling and simulation tools will be employed to design lattice structures (e.g., a gyroid structure) that reduce stress concentrations and thus increase fatigue resistance, and (3) one-dimensional (1-D) carbon nanotubes will be added to enhance radiation resistance. To validate our solution, high-temperature tensile and fatigue testing, in combination with microstructure characterization, will be conducted on wrought materials, additively manufactured solid materials, and the designed lightweight lattice structure material. Ion irradiation, microstructure characterization, and nanoindentation will be carried out to investigate the effect of 1-D carbon nanotubes on radiation tolerance. Successful completion of this project will deliver a material to serve as a substitute for current SS316 using the same chemistry but with lighter weight and improved mechanical properties. In addition, a material with carbon nanotubes can be designed for improved radiation tolerance over a suitable service temperature range. This project will establish new techniques in innovative materials/lattice design, advanced macroscale properties prediction, and the application of state-of-the-art processes.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Initial ASME code rule analysis on Simple and Full assessment

ASME & ASTM codes present simple and full assessment methodologies to qualify nuclear grade graphite components. This report explains the theory behind the statistical portion of the codes and describes the issues discussed in a 2020 workshop in the simple assessment, as well as the full assessment. The methodology for the full assessment was developed by Hindley []. He used a validation methodology to match the experimental average failure load of test specimens from several geometries to the calculated 50% POF load to tune the grouping criteria parameters based on an RMSE penalty function. The grouping criteria consists of a minimum volume to satisfy the weakest link theory of the Weibull distribution and a minimum stress range parameter. Hindley’s work found a minimum link volume of 10 times the grain size and a stress range parameter of 7% [satisfy the validation requirements. Several studies found that the link volume of 10 times the grain size was not satisfactory for the volume grouping criteria for graphite grades with fine grains. ASME 2021 code adopted a new volume grouping criteria based on fracture toughness for calculation of the process zone volume. However, errors were found in the ASME 2021 code process zone volume equation and the question is now open as to what volume grouping criteria is satisfactory. This report presents results from sensitivity studies that were done to evaluate the volume grouping criteria effect on the full assessment POF. This report also presents results from sensitivity studies on other aspects of the code that affect the POF, the mesh size and the choice of the Weibull threshold parameter. All three sensitivity studies: the volume grouping criteria, the mesh size, and the threshold parameter choice are found to affect the component qualification decision for components of structural reliability class 1 (SRC-1). The sensitivity analysis results are presented in the body of the report for NBG-18, which is the same grade of graphite as Hindley used in his thesis. Results from NBG-17, IG-110, 2114, and PCEA are presented in the Appendix. For NBG-18, it was found that increasing the threshold increases the POF, finer meshes result in higher POFs, and that smaller link volume requirements lead to higher POFs (which is inconsistent with Hindley’s findings). This report proposes a new validation study similar to Hindley’s []. The purpose of the new validation study is to tune the threshold, mesh size and grouping criteria based on results from multiple grades of graphite, including finer grain graphites T220 (1-3 microns) and NG-CT-50 (5 microns). The test specimens will be broken at 3 labs, such that we can measure between lab measurement variability, with at least 5 test specimens per lab such that the within lab uncertainty can also be measured. Hindley’s validation method tried matching the average experimental load with the median. The future study will attempt to match failures at lower percentiles, which would be closer to the SRC POF limit. We are currently looking into what geometries make sense and the best method to measure multi-axial stress states. These design decisions are still being set.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Water-Weakening and Time-Dependent Deformation of Organic-Rich Chalks

Abstract The Ghareb Formation is a shallowly buried porous chalk in southern Israel that is being considered as a host rock for a geologic nuclear waste repository. Setup and operation of a repository will induce significant mechanical, hydrological and chemical perturbations in the Ghareb. Developing a secure repository requires careful characterization of the rock behavior to different loads. To characterize hydromechanical behavior of the Ghareb, several short- and long-term deformation experiments were conducted. Hydrostatic loading tests were conducted both dry and water-saturated, using different setups to measure elastic properties, time-dependent behavior, and permeability. A set of triaxial tests were conducted to measure the elastic properties and rock strength under differential loading at dry and water-saturated conditions. The hydrostatic tests showed the Ghareb began to deform inelastically around 12–15 MPa, a relatively low effective pressure. Long-term permeability measurements demonstrated that permeability declined with increasing effective pressure and was permanently reduced by ~ 1 order of magnitude after unloading pressure. Triaxial tests showed that water saturation significantly degrades the rock properties of the Ghareb, indicating water-weakening is a significant risk during repository operation. Time-dependent deformation is observed during hold periods of both the hydrostatic and triaxial tests, with deformation being primarily visco-plastic. The rate of deformation and permeability loss is strongly controlled by the effective pressure as well. Additionally, during holds of both hydrostatic and triaxial tests, it is observed that when water-saturated, radial strain surpassed axial strain when above effective pressures of 13–20 MPa. Thus, deformation anisotropy may occur in situ during operations even if the stress conditions are hydrostatic when above this pressure range.

58 GEOSCIENCES↗

DOE OSTI2025

Multigene engineering in plants: Technologies, applications, and future prospects

The emerging bioeconomy presents a promising solution to both economic and environmental challenges. Within the bioeconomy, plants serve as a renewable, sustainable, and cost-effective source of foods, fuels, chemicals, and materials. However, traditional breeding and single-gene engineering approaches fall short in addressing complex traits (e.g., drought tolerance, disease resistance, yield, nutrient use efficiency) which are controlled by multiple genes. The complexity of plant biology often necessitates the use of multigene engineering (MGE), which involves simultaneous ectopic expression, up/down-regulation, or editing of multiple genes, to enhance plant traits relevant to the bioeconomy. These genes may be associated with distinct traits or function as components of specific metabolic and regulatory pathways. This review summarizes current technologies for MGE within the synthetic biology-driven Design-Build-Test-Learn (DBTL) framework, detailing its four key stages: Design – gene construct development; Build – DNA assembly and plant transformation; Test – the molecular, biochemical, and physiological characterization of engineered plants; and Learn – computational modeling to refine, multiplex and iterate the process. Despite good progress in the applications of MGE in biofortification, metabolic engineering, and stress resilience, challenges remain in construct stability, coordinated gene expression, and regulatory predictability. We identified optimization paths and future directions to accelerate MGE deployment in sustainable agriculture, with possible societal benefits including reduced production costs, increased yield, and improved food and nutritional security.

AI-aided plant engineering↗

DOE OSTI2020

Influence of plasticizers on thermal and mechanical properties of biocomposite filaments made from lignin and polylactic acid for 3D printing

Polylactic acid (PLA) and organosolv lignin were mixed at different ratios and extruded to obtain PLA-lignin composite filaments. PLA was replaced with lignin up to 20 wt%. Two plasticizers (polyethylene glycol (PEG) 2000 and struktol TR451) were added in varying concentrations to enhance the properties of PLA_L20 (20% lignin in PLA) composite filaments. Furthermore, the effect of lignin in PLA, and PEG, and struktol in PLA_L20 composites was investigated via tensile test, differential scanning calorimetry, thermogravimetric analysis, scanning electron microscopy, Fourier transform infrared spectroscopy of the filaments, and dynamic mechanical analysis of 3D printed samples. A 2 wt% PEG was able to enhance both tensile stress and elongation at maximum load of PLA_L20 composite by 19% and 35%, respectively, whereas struktol TR451 was able to improve elongation at maximum load by 24%.

3D printing↗

DOE OSTI2020

Fracture toughness evaluation for thin-shell stainless steel weldment

Integrity of spent nuclear fuel (SNF) interim storage canisters are very important to the safety of the back-end nuclear fuel cycle. Stress corrosion cracking (SCC) potential of interim storage canister has been considered as a high priority. Because no post-weld heat treatment was required for forming these canisters, the high tensile residual stress existed within these canister welds. This can change the fracture resistance capacity significantly as well as increase SCC potential. Due to relative thin shell thickness of a canister weldment, the spiral notch torsion test (SNTT) method of small specimen approach was used to estimate the canister weldment fracture toughness. Most SNTT weldment samples fracture initiation sites are at heat-affected zone (HAZ) regions. The estimated fracture toughness $J_Q'$ for the baseline SS304 steel is at 283 kJ/m 2 . The estimated $J_Q'$ for the SS304/308 weld from HAZ and weld specimens are 126 kJ/m 2 and 148.9 kJ/m 2 , respectively.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Tribocatalytically-activated formation of protective friction and wear reducing carbon coatings from alkane environment

Minimizing the wear of the surfaces exposed to mechanical shear stresses is a critical challenge for maximizing the lifespan of rotary mechanical parts. In this study, we have discovered the anti-wear capability of a series of metal nitride-copper nanocomposite coatings tested in a liquid hydrocarbon environment. The results indicate substantial reduction of the wear in comparison to the uncoated steel substrate. Analysis of the wear tracks indicates the formation of carbon-based protective films directly at the sliding interface during the tribological tests. Raman spectroscopy mapping of the wear track suggests the amorphous carbon (a-C) nature of the formed tribofilm. Further analysis of the tribocatalytic activity of the best coating candidate, MoN-Cu, as a function of load (0.25–1 N) and temperature (25 °C and 50 °C) was performed in three alkane solutions, decane, dodecane, and hexadecane. Results indicated that elevated temperature and high contact pressure lead to different tribological characteristics of the coating tested in different environments. The elemental energy dispersive x-ray spectroscopy analysis and Raman analysis revealed formation of the amorphous carbon film that facilitates easy shearing at the contact interface thus enabling more stable friction behavior and lower wear of the tribocatalytic coating. These findings provide new insights into the tribocatalysis mechanism that enables the formation of zero-wear coatings.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Power Plant Testing of Ultrasonic Measurements of Temperature Distributions and Heat Fluxes to Heat Exchange Surfaces

Extreme environmental conditions are common in energy conversion applications, in which the most hardened insertion sensors often do not perform reliably for long. On the other hand, ultrasonic measurements can be acquired noninvasively, with sensitive components kept away from the damaging environment. We have previously developed the ultrasonic method for measuring the spatial distribution of temperatures in solid materials applicable when large thermal gradients are present. In the developed approach, we use the echogenically segmented ultrasound propagation path, structured to contain engineered or naturally occurring echogenic features, to produce a train of echoes in response to an external pulse of ultrasonic excitation. This paper outlines the testing results of this approach applied to the temperature distribution measurements to a waterwall of a 500 MW power-plant utility boiler. The validation results obtained over the prolonged power plant test show that the estimated temperature profile is correctly captured, and the measurement accuracy can be comparable with traditional insertion sensors, such as thermocouples. Overall, the testing has confirmed that the developed approach has matured to become an attractive alternative to conventional sensing in solving challenging problems of long-term temperature measurements in extreme environments. Heat fluxes and thermal stresses in the structure can then be characterized noninvasively using the measured temperature distribution as the basis.

Walton, Kenneth↗

DOE OSTI2019

Ultrasonic Measurements of Temperature Distribution and Heat Fluxes Across Containments of Extreme Environments

Extreme conditions are common in energy conversion, material processing, nuclear, airspace, and military applications. In such environments, the most hardened insertion sensors do not perform reliably for long. Ultrasonic measurements, on the other hand, can be acquired noninvasively, with sensitive components kept away from the damaging environment. We have previously developed the ultrasonic method for measuring the spatial distribution of temperatures in solid materials applicable in the cases when large thermal gradients are present. In the developed approach, we use the echogenically segmented ultrasound propagation path, structured to contain engineered or naturally occurring echogenic features, to produce a train of echoes in response to an external pulse of ultrasonic excitation. The delays between the echoes, which encode the information on the temperature distribution in the corresponding segments, is used to reconstruct unknown temperature profile. In this paper, we outline the results of pilot-scale testing of the developed approach and demonstrate its application to the measurements of the temperature distribution across the containment of a high-temperature combustion process. The validation results show that the estimated temperature profile is correctly captured, and the measurement accuracy can be comparable with traditional insertion sensors, such as thermocouples. Overall, the testing has confirmed that the developed approach has matured to become an attractive alternative to conventional sensing in solving challenging problems of long-term temperature measurements in extreme environments. Heat fluxes and thermal stresses in the structure can then be characterized noninvasively using the measured temperature distribution as the basis.

Jia, Yunlu↗

DOE OSTI2024

Utah FORGE: Direct Shear Test Data for Investigating Seismic Precursors to Shear Failure of Fractures

This dataset includes results of direct shear tests to investigate the mechanical and geophysical response of dry and saturated fractures in Indiana limestone and Sierra White granite. Direct shear tests were performed on tensile-induced fractures in Indiana limestone and Sierra White granite in a custom water-pressurized chamber. The provided Excel files include the representative seismic wave signals and the normalized wave amplitudes of ultrasonic wave transducers. A link to the published journal article presenting the data and describing the experiment in detail is provided as well.

15 GEOTHERMAL ENERGY↗

DOE OSTI2021

Field Experiments and Model Validation: The EGS Collab Project

Implementing enhanced geothermal systems (EGS) will require improvements in understanding stimulation of crystalline rock to create appropriate flow pathways, and the ability to effectively simulate both the stimulation and the flow and transport processes in the resulting fracture network. The US Department of Energy (DOE) is addressing these and other challenges at multiple scales. The EGS Collab project, addressed here, is performing tests and modeling at the 10 m scale. The FORGE project is performing tests at the full reservoir scale. The EGS Collab team created an underground testbed at the Sanford Underground Research Facility (SURF) in Lead, South Dakota, at a depth of approximately 1.5 km to examine hydraulic fracturing (Experiment 1). We are currently building a second testbed at SURF at a depth of about 1.25 km aimed at investigating shear stimulation (Experiment 2). In Experiment 1, we drilled eight boreholes in a well-characterized phyllite and installed geophysical sensors in six of them to create a well-instrumented testbed to allow careful monitoring of stimulation events and flow tests. Numerical simulation was used to answer key experimental design questions, to forecast fracture propagation trajectories and extents, and to analyze and evaluate results both in near-real-time and in detailed process studies. Stimulations performed in this testbed allowed quantification of processes occurring during stimulation and the examination of dynamic flow occurrences. Long-term ambient temperature and chilled water flow tests were performed in addition to many tracer tests to examine system behavior. Our second testbed, targeted at shear stimulation, is currently being built at the SURF Facility at a depth of about 1.25 km in amphibolite under a different set of stress and fracture conditions than Experiment 1.

artificial intelligence↗

DOE OSTI2021

Durability of plasma sprayed Thermal Barrier Coatings with controlled properties part Ⅱ: Effects of geometrical curvature

The present investigation elucidates the effects of substrate curvature on the durability of Air Plasma Sprayed (APS) Thermal Barrier Coatings (TBCs). Traditionally, planar disk specimens are utilized in Furnace Cycle Testing (FCT). In most cases, delamination is initiated at the disk's free edge and then propagates along the TBC-bond coat interface. However, in turbine components (e.g., blades/vanes), they lack significant free edges and the coatings are deposited on non-flat surfaces of varying radii of curvature. These geometrical discrepancies imply significant differences in the stress states as compared to planar disk specimens. Therefore, the part geometry inevitably affects the TBC failure mechanisms in the turbine system, and consequently influences TBC durability. Nevertheless, these effects have not been fully explored in the past, despite the anecdotal knowledge which suggests the leading edge of turbine blades to be one of the most common failure/spallation locations. Here in this study, representative TBC systems were deposited onto superalloy disks with flat substrate and rods with curved substrate. The experimental results from FCT suggest TBC durability on rods is significantly lower than when sprayed on disks. Furthermore, the durability of TBCs on rods appears to increase with higher porosity, which is contradictory to reported trends for TBCs on disks. In addition, the effects of various bond coats are not consistent with those observed in disks. To clarify the underlying effects of curved geometries, detailed stress analyses were performed. They revealed a state of thermal stresses which is unique to curved geometries. It was found that TBC on rods experience tensile radial stresses as well as tensile hoop stresses during the cooling. These stresses result in a complex interplay in failure processes in rods, which explains the different observed trends in the durability from those obtained with disks.

36 MATERIALS SCIENCE↗

DOE OSTI2024

In-service Oxidation and IASCC in High Fluence Baffle-Former Bolts Retrieved from a Westinghouse PWR

Baffle-former bolts (BFBs) are subjected to significant mechanical stress and neutron irradiation from the reactor core during the plant operation. Over the long operation period, these conditions lead to potential degradation and reduced load-carrying capacity of the bolts, and life extension of existing pressurized water reactors (PWRs) would only cause more damage to the bolt material. To this end, the Light Water Reactor Sustainability (LWRS) Program Materials Research Pathway (MRP) successfully harvested two high fluence BFBs from a Westinghouse two-loop downflow type PWR in 2016. In the same year, the two BFBs were received at the Westinghouse Churchill facility for inspection and specimen fabrication. The fabrication was completed in 2017 with specimens shipped to Oak Ridge National Laboratory (ORNL) for further testing. The objective of this project is to provide information that is integral to evaluating end of life microstructure and properties as a benchmark of international models developed for predicting radiation-induced swelling, segregation, precipitation, mechanical property degradation, and with the latest findings, susceptibility to irradiation-assisted stress corrosion cracking (IASCC).

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2023

In-situ determination of moisture- and temperature-driven deflection of an encapsulated Si photovoltaic cell

Module reliability and service lifetime are critical factors in improving photovoltaic system performance and reducing the levelized cost of electricity (LCOE). Soldering and lamination of the cell impart residual stresses that persist over time and superimpose additional loads during operation. This paper demonstrates the use of X-ray Topography (XRT) to image in-situ the dynamic response of a glass/backsheet mini-module upon drying at elevated temperature after saturation at humidity levels compatible with accelerated testing. The local water content in the encapsulant is also determined in-situ over time via Water Reflectometric Detection (WaRD), with diffusion of water in the front (glass side) and rear (backsheet side) resolved. As water diffuses out from the back of the glass/backsheet module, the cell curves towards the backsheet concomitantly. Here we find that the cell edges deflect 40μm out-of-plane with respect to its center while the encapsulant dries, compared to ~100 μm deflection when heating from 25°C to 85°C. The local cell deflections (changes in cell orientation) are correlated with the dynamic loss of water in the backside encapsulant. We conclude that the observed cell deflections are the result of hygroscopic stress induced by the encapsulant upon moisture outdiffusion. Therefore, the cell experiences a continually changing stress state and curvature dependent on local humidity and temperature. Depending on cell architecture and interconnection, this “breathing” mode of the cell may induce wear out and fatigue of the interconnects, affect the electrical connection of cracked pieces or cause failure near the interconnected edges of two cells.

14 SOLAR ENERGY↗

DOE OSTI2024

A high-resolution pseudo-polygon discrete element model for regional sea ice

Here, this work presents a pseudo-polygon discrete element model for high-resolution sea ice simulations. A scale-invariant bonded particle contact model is proposed to model joints between sea ice floes based on the smeared fracture model and a lattice spring beam model, and the Mohr–Coulomb failure criterion is implemented to represent the shearing failure mechanism of sea ice packings under complex loadings. All mechanical parameters of the bond model can be directly determined from laboratory tests. Validations of the proposed model are made by investigations of mechanical response and failure criteria of field sea ice sheets. Compared with the field observations of sea ice from satellite radar and in situ stress sensors, the proposed model is capable of reproducing the typical constitutive behavior and the Coulomb friction envelope of field sea ice. Finally, the proposed discrete element sea ice model is used to study the effect of loading rates on mechanical behavior including failure strength of regional sea ice.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2025

Temperature and Strain Sensing Characteristics of a 128° YX-Cut LiNbO 3 Rayleigh-Mode SAW Sensor From Room to Cryogenic Temperatures

Accurate, passive, and wireless monitoring of cryogenic hardware is essential for high-energy physics, space propulsion, and biomedical instrumentation. Here, this study quantifies the coupled temperature-strain behavior of Rayleigh-mode surface acoustic-wave (SAW) delay-line sensors fabricated on 128° YX-cut LiNbO 3 . A nonlinear finite element (FE) model incorporating Varshni-based elastic constants, higher-order thermal expansion, and temperature-dependent piezo- and dielectric coefficients was developed and validated experimentally between 280K and 80K. Free-standing (first test condition) and bonded/wired (second test condition) devices exhibited indistinguishable thermal responses; the average temperature coefficient of delay (TCD) in the critical cryogenic range from 130K down to 80K differed by only 0.15 ppm/K (0.32%), confirming that bonding-induced stress is negligible. Over 280-80K the measured TCD was 61.77 ppm/K, while the FE model predicted an equivalent temperature coefficient of frequency (TCF) of −62.74 ppm/K with an overall coefficient of determination R2 = 0.998. In the critical cryogenic interval 130-80K the TCD fell to 47.66 ppm/K, indicating improved thermal stability at low temperature. Controlled loading (0-300 με) revealed a strain coefficient of delay (SCD) that rises from 0.53 ± 0.02 ppm/με at 300K to 1.05 ± 0.02 ppm/με at 80K. This modest sensitivity confirms that, for temperature sensing, strain is a second-order perturbation above 135K but must be compensated at deeper cryogenic levels. Overall, this work establishes a predictive multiphysics model together with repeatable wired measurements that confirm the suitability of SAW sensors for temperature and strain monitoring in extreme cryogenic environments, while also providing a baseline for future wireless implementations.

25 ENERGY STORAGE↗