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DOE OSTI2020

Addition of Chloroform in a Solvent-in-Salt Electrolyte: Outcomes in the Microscopic Dynamics in Bulk and Confinement

Solvent-in-salt electrolytes (SISEs) are a promising alternative to the electrolytes currently used in commercial devices. Despite the SISEs’ advantages, their utilization is not yet realized due to the poor mobility of their chemical species. Here, we explore this problem by adding chloroform to a SISE formed by acetonitrile and a Li-salt. First, we performed illustrative cycling experiments to highlight the potential of this approach. Then, we focused on the description of the microscopic dynamics of the electrolytes and exposed the relevant aspects to be considered for their optimal performance. While the conductivity at low temperatures may be enhanced by the addition of chloroform, only subtle changes occur at room temperature. As revealed by molecular dynamics simulations and quasielastic neutron scattering (QENS) experiments, this effect is related to the preservation of the structure expected for a highly concentrated solution and promotion of the formation of ionic aggregates. These outcomes occur despite the increase in the overall mobility of the chemical species. The dynamics of the electrolytes in porous carbon was also investigated using QENS. In these circumstances, low concentrations of chloroform lead to diffusivities of the molecular species higher than those observed for the bulk electrolytes. As chloroform’s concentration increases, no further changes in the diffusivities are observed. Nonetheless, chloroform is mostly immobilized on the carbon surfaces and this behavior may be intensified at compositions closer to the eutectic mixture.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Quantifying Properties for a Mechanistic, Predictive Understanding of Aqueous Impact on Aging of Medium and Low Voltage AC and DC Cabling in Nuclear Power Plants

To address the gap in knowledge in understanding degradation in relevant service conditions, this project aimed to develop a mechanistic, predictive model of medium and low voltage cable failure based on the primary environmental degradation parameters of aqueous immersion time, temperature, and the oxidation extent. To do so, we took a two-fold approach toward evaluating degradation as related to the aqueous condition. First, we evaluated the chemical, mechanical, and electrical properties of polymers that comprise the cabling insulation under varied aqueous conditions at different temperatures. Secondly, we evaluated the performance of insulation materials under similar accelerated aging conditions in addition to the dielectric breakdown of the cabling under submersion conditions. Thermal oxidation and immersion of LDPE thin films were done using a Parr vessel and the extent of oxidation was monitored using the carbonyl index from ATR-FTIR spectrum, a ratio quantifying the carbonyl functionality produced on the LDPE film surface. Increasing the temperature, oxidation time, and oxygen pressure increased the water-vapor permeability and the carbonyl content. Thermogravimetric analysis of the films confirmed that there is indeed an initial weight loss of the smaller molecular weight molecules and volatiles. At higher temperatures, there is a secondary mass loss. Up to 70°C, the mass loss curves were similar until 80°C, when the aged films decreased at a much greater rate with respect to increasing temperature. This was seen in the 10, 50, 90% weight loss temperatures. The mechanical properties of sheet PP and HDPE as well as injection molded LDPE, HDPE, HDPP dog bones were plotted with respect to the time spent in the Parr vessel during thermal oxidation. For the sheet PP and HDPE, the UTS and the modulus of elasticity decreased while the elongation increased. The injection-molded LDPE, HDPE, and HDPP dog bones experienced a similar trend where the changes in the properties were within experimental uncertainty. This analysis of LDPE in dry and immersive oxygen-rich environments is an important baseline for future experiments looking at other degradation mechanisms. A predictive aging model for low-density polyethylene insulative cable housings was developed. This model revealed a combination of physical and chemical processes which lead to an increase in permeability and a decrease in strength of the insulator. In creating this predictive model, a gap of knowledge in the literature was revealed in two areas: understanding how the crystallinity of a polymer changes with time and visualizing the predicted pores formed through the insulator which leads to failure. Developing and using an adapted ATR-FTIR method, crystallinity was monitored and compared to bulk crystallinity found via DSC. Inhomogeneity in crystallinity changes were observed but the FTIR method but was found to be less reliable. Pore visualization was found utilizing electrical impedance spectroscopy saturated aged polyethylene films with synthesized citrate-capped gold nanoparticles, and chloroauric acid precursor. results indicate a decreasing impedance of the polyethylene films caused by the transport of ions through the film. SEM imaging was then performed for elemental analysis of the films and counter electrodes for the presence of ions. Chloride and gold ions were detected; however, no nanoparticles were found. This gives an estimated pore size of at least 0.3 nm through the aged film. Cyclic submergence of polyethylene and polypropylene in aqueous solutions of copper sulfate and Harrison’s solution were examined. It was discovered that aging in these mixed conditions and at 90°C did cause a small, yet significant increase to tensile strength for both unaged polyethylene and polypropylene. The PE and PP in cycled and submerged conditions did not have tensile strengths significantly different from dry-aged after 16 weeks. For both solutions, it was determined that capacitance increases with both water tree depth and cable temperature and is relatively independent of changing water tree AR. As for resistance, there is no apparent change between depth percentages of 10 and 80 for both solutions. This is because the water tree has not yet entered the conductor and thus there is no shorting current flowing through the tree yet. Between 80 and 100% water tree depth, it is observed that for both solutions there is a rapid decrease in resistance because the tree is now impacting the conductor shield and allowing shorting current to flow through it. The relationship between resistance and temperature was found to be inversed. As temperature increases, resistance decreases for both water tree solutions with distilled water having the most apparent difference across the range of temperatures simulated. With regards to water tree AR, resistance was found to be relatively independent at depth percentages of 10, 50, and 70, but there was some relationship at 100% depth for both solutions. At this depth, as water tree AR increased, resistance was found to also increase. Through the examination of voltage and electric field distribution plots, it was confirmed for EPR cables that increasing water tree depth leads to increasing distortion. The increase in shorting current at 100% depth for aqueous copper sulfate compared to distilled water was also visualized. Lastly, the relationship between shorting current and temperature for narrow water trees was visualized and validated using the distribution plots. This study has led to a better understanding of the effect of cable temperature, water tree solution, and geometry of the tree region on cable degradation. Furthermore, this study has documented simulation results of water tree degradation in EPR MV cables, which had been previously lacking in information. Future work in this area will add frequency into the mix and examine what effect it has on the rate of cable degradation as a result of water treeing. To compliment the work being carried by UMD on different polymer chemistries, harvested medium voltage (MV) cables were selected for accelerated aging study at ORNL. These medium voltage cables are representative of the vintages and materials that are currently in use at existing nuclear power plants (NPPs). These cables were immersed in water at 90°C and energized for a period of two years at elevated voltage. Partial discharge was measured during this period of time to track potential degradation. Unfortunately, due to the absence of failure, the extent of integration between the UMD techniques and the harvested MV insulation was limited. However, based on the findings and from the UMD research in the previous sections on polyethylene and polypropylene, follow-on characterization for harvested MV cable insulation should focus on sample preparation to take advantage of the UMD techniques to better understand mechanistic degradation in MV cable insulations. This would include: 1.) Utilization of solutions and impedance measurement insulation to track permeability in harvested and accelerated aging insulation samples, 2.) Adaptation of gold nanoparticle synthesis for electrical impedance spectroscopy with supporting SEM characterization to study pore formation in harvested and accelerated aged insulation samples, & 3.) ATR-FTIR crystallinity with multiple temperature dependent harvested MV cable insulation under different air and submerged accelerated aging. In addition, low voltage dielectric spectroscopy and high voltage dissipation factor, tan δ, could be implemented as a condition monitoring tool for harvested MV cable insulation in submerged environments.

24 POWER TRANSMISSION AND DISTRIBUTION↗

DOE OSTI2024

Synthesis, Processing, and Use of Isotopically Enriched Epitaxial Oxide Thin Films

Isotopic engineering has emerged as a key approach to study the nucleation, diffusion, phase transitions, and reactions of materials at an atomic level. It aims to uncover mass transport pathways, kinetics, and operational and failure mechanisms of functional materials and devices. Understanding these phenomena leads to deeper insights into important physical processes, such as the transport of ions in energy conversion and storage devices and the role of active sites and supports during heterogeneous catalytic reactions. Likewise, isotopic engineering is being pursued as a means of modifying functionality to enable future technological applications. In this Account, we summarize our recent work employing isotope labeling (e.g., 18 O 2 and 57 Fe) during thin film synthesis and postgrowth processing to reveal growth mechanisms, defect chemistry, and elemental diffusion under working and extreme conditions. Isotope-resolved analysis techniques with nanometer-scale spatial resolution, such as time-of-flight secondary ion mass spectrometry and atom probe tomography, facilitate the accurate quantification of isotopic placement and concentration in our well-defined heterostructures with precisely positioned, isotope-enriched layers. By measuring the nanometer-scale redistribution between natural abundance and isotopically enriched oxygen layers during the deposition of Fe 2 O 3 and Cr 2 O 3 by molecular beam epitaxy, we identified intermixing processes driven by surface adatoms occurring both at the film growth surface and within the first few layers below the surface. Further insights into synthesis mechanisms were gained by studying the tungsten oxide thin films grown by evaporating WO 3 powder in the presence of background 18 O 2 , revealing minimal incorporation of background oxygen during the film formation process. Thermal and radiation-enhanced diffusion in epitaxial Fe and Cr oxides were precisely tracked using 18 O and 57 Fe tracer layers incorporated into model epitaxial oxide thin films. This approach has allowed us to access thermal diffusion behavior at lower temperatures than previously measured, revealing a potential changeover in diffusion mechanism. Understanding radiation-enhanced diffusion in model oxides that represent the surface layers on the structural components of nuclear reactors informs our understanding of their corrosion behavior under irradiation. Isotopic labeling can also provide unique insights into the surface exchange reactions and defect chemistry of electrocatalysts. For instance, tracking the change in 18 O concentration at the surface of an epitaxial LaNiO 3 thin film after the electrocatalytic oxygen evolution reaction revealed the participation of lattice oxygen, confirming a hypothesis that had been proposed previously. Lastly, we highlight a new direction wherein we perform in situ processing studies utilizing isotopic tracers in conjunction with model epitaxial thin films within the atom probe tomography instrument. Additionally, this Account illustrates the great potential of isotopic engineering to enable fundamental mechanistic insights into physical processes and engineer functional properties in epitaxial films, heterostructures, and superlattices.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Onshore U.S. Carbon Pipeline Deployment: Siting, Safety, and Regulation

Carbon capture, utilization, and storage (CCUS) technology has significant potential to reduce greenhouse gas (GHG) emissions and mitigate the impact of climate change, particularly in hard to decarbonize industrial and commercial sectors. CCUS involves capturing carbon dioxide (CO 2 ) from industrial processes or power generation and utilizing it for other purposes, such as enhanced oil recovery (EOR), or storing the captured CO 2 underground. CCUS technology can reduce the environmental impact of continued fossil fuel use while smoothing the transition to a low-carbon economy. CCUS can create new economic opportunities, such as the development of new industries and job creation, and can enhance energy security by diversifying energy sources. For these reasons, enabling CCUS has become a key objective of the Biden-Harris administration’s clean energy policy and has received bipartisan support. Despite its environmental and economic potential, CCUS faces multiple barriers to widespread deployment. One of the main challenges is the high cost and technical difficulty of implementing and operating large-scale CCUS infrastructure. CCUS remains a relatively expensive way to reduce carbon emissions (e.g., compared to solar photovoltaic technology’s displacement of coal generation). Additionally, financial incentives and supportive policies like those enacted to support solar photovoltaic development, especially at the state level, are inconsistent or nonexistent, which can discourage investment in CCUS projects. There are also technical challenges associated with safe and secure underground CO 2 storage and the development of new carbon utilization technologies. Public opposition to various aspects of CCUS technologies, ranging from concerns that CCUS will extend reliance on fossil fuels to CCUS infrastructure being sited in disadvantaged communities, is a growing challenge. This paper focuses on another significant barrier to broad CCUS deployment: the need for considerable expansion of the dedicated land-based CO 2 pipeline network in the United States to meet CCUS goals and the unique regulatory challenges to its development. To reach carbon emissions targets in the United States by 2050, CCUS technology will need to be supported by tens of thousands of miles of CO 2 pipelines. Estimates range from a minimum of roughly 29,000 pipeline miles (according to a 2020 Great Plains Institute study) to 66,000 pipeline miles (as per a 2021 Princeton University–led study). As of October 2022, however, the U.S. Department of Transportation (U.S. DOT) reports fewer than 5,400 miles of U.S. pipelines carrying CO 2 . This deficit—and what it means for the prospect of moving substantially larger quantities of CO 2 from source to use or storage—threatens to stifle the development of CCUS projects and technologies identified as an important tool to meet emissions targets. The current regulatory landscape facing CO 2 pipeline development can best be described as uncertain. At the federal level, the U.S. DOT Pipeline and Hazardous Materials Safety Administration (PHMSA) oversees safety regulation of pipelines transporting hazardous materials, including CO 2 upon commencement of operation. However, PHMSA’s definition of CO 2 as “a fluid consisting of more than 90 percent CO 2 molecules compressed to a supercritical state” has not been updated since its 1991 addition to the Federal Register. Because CO 2 can be transported in a gaseous, liquid, or supercritical state (indeed, the physical state of CO 2 can fluctuate within a single pipeline due to environmental changes), doubts persist about the extent of PHMSA’s purview—and raise questions about what, if anything, states should do to address this apparent gap. PHMSA has begun a major revision of its existing rules, but the agency does not expect a first draft before 2024. Economic oversight of CO 2 pipelines is even less clear. The Federal Energy Regulatory Commission (FERC) and Surface Transportation Board (STB)—which regulate the rates of interstate oil/natural gas and non-energy pipelines, respectively—have both declined jurisdiction over interstate CO 2 pipelines. This presumably leaves economic regulation to state and/or local governments, but few if any states have the laws or resources in place to oversee just and reasonable rates. Further, the interstate nature of CO 2 pipeline development creates questions around how different states should align their rate-making decisions. Onshore U.S. Carbon Pipeline Deployment: Siting, Safety, and Regulation Currently, regulatory responsibilities regarding CO 2 pipeline siting and permitting fall to state and local governments. The variety of laws and regulations across the country, however, creates a maze of requirements for pipeline developers to navigate. To secure necessary permits, most states require pipeline companies to be “common carriers” that provide transport service to the public at uniform rates. However, the specific definition of that term varies. Some states require clear evidence that a pipeline services the public, while others automatically deem any pipeline company transporting energy products or hazardous materials to be a “common carrier”—with little consideration for accessibility to third parties. Other states have eschewed common-carrier terminology entirely, placing private and publicly accessible pipelines on equal footing. Much like the variation in common-carrier requirements, laws governing eminent domain authority to secure rights-of-way (ROW) to commence construction on a planned pipeline route differ by state. Several states have no laws or rules governing CO 2 pipelines. In addition to creating questions about whether long-standing rules for other pipelines (e.g., natural gas or petroleum products) apply to CO 2 , this policy vacuum leaves local governments as the sole authority over sections of pipe within their boundaries. With dozens of counties along a given route, the probability of inconsistent regulation of the same pipeline is significant. Even in states with CO 2 pipeline laws in place, local regulatory attempts to address rising concerns over pipeline routing and safety have triggered lawsuits by pipeline companies seeking to delimit areas of federal, state, and local government responsibility. Meanwhile, legislators across the country have introduced bills to restrict the application of eminent domain to CO 2 pipeline projects, which could threaten a key means of securing ROW that companies cannot secure through negotiation with landowners. Taken separately, any of these regulatory issues—the narrow federal definition of CO 2 , FERC’s and STB’s decisions that CO 2 pipelines are not within their jurisdiction, and the considerable variation in state and local governments’ laws regulating CO 2 pipeline technologies—are extremely difficult to resolve. Adding the required scale of CO 2 pipeline expansion and the currently identified narrow window of time in which to reach climate target goals, the task becomes even more difficult—and raises a host of urgent questions for regulators. How should CO 2 be defined in federal regulations to ensure consistent safety standards across the country? What is the potential impact radius of a CO 2 pipeline rupture, and how should that inform local emergency response? In the absence of centralized federal oversight, what should state legislatures do to increase alignment for interstate CO 2 pipeline projects? This paper intends to serve as a primer for regulators and stakeholders who seek to better understand the regulatory challenges and opportunities facing this critical infrastructure.

42 ENGINEERING↗

DOE OSTI2024

A Review of Modeling Approaches for Predicting Frost Growth and Defrosting on Tube-Fin Heat Exchangers: Preprint

Frost formation and growth on the evaporator surface is a common process that deteriorates the air-refrigerant heat transfer and restricts airflow. This degrades the performance of the vapor compression system by increasing temperature lift and air-side pressure drop. To accurately predict these effects during coil frosting, as well as the energy use and duration of the defrost process, there is a need to estimate the heat and mass transfer, momentum transport, and solid-liquid and liquid-vapor phase change. Therefore, in the past few decades, continuous effort has been made to model frosting and defrosting processes using approaches ranging from empirical correlations to computational fluid dynamic models. To provide a clearer overview for researchers, engineers, and manufacturers in this field, this paper provides a comprehensive literature review for frosting and defrosting models. The paper begins with theoretical background of frost formation and defrost processes, and then reviews the common modeling approaches in literature and their underlying assumptions when trying to account for various physical phenomenon. Based on the literature review, the most critical modeling effort for frost formation is the determination of frost densification rate and frost growth rate. Various methods to predict these two parameters are reviewed. Empirical correlations commonly used for frost density and thermal conductivity are presented and compared. For the defrost process, various multi-stage models have been proposed with different assumptions. Some assume the presence of air gap between the tube wall and the frost, while others consider the melted frost flow due to gravity. We also review physics-based and empirical approaches to integrate defrost models into heat pump models. We conclude by identifying research gaps and providing recommendations.

defrost↗

DOE OSTI2020

Subtask 1.3 – Integrated Carbon Capture and Storage for North Dakota Ethanol Production

The Energy & Environmental Research Center (EERC), in partnership with Red Trail Energy, LLC (RTE), a North Dakota ethanol producer; the North Dakota Industrial Commission (NDIC) Renewable Energy Program (REP); and the U.S. Department of Energy (DOE), conducted a feasibility and implementation study for a commercial carbon capture and storage (CCS) effort. This subtask provided technical support and developed recommended practices of how small-scale industrial CO2 emitters (<1,000,000 tonnes of CO2 emitted annually) may economically deploy CCS. The 64-million-gallon dry mill RTE ethanol facility, emitting an average 180,000 tonnes of CO2 annually, was the subject of the case study. The positive outcome of this research, which shows technical and economic potential for ethanol–CCS in North Dakota, has resulted in RTE acquiring an approved Permit to Drill on December 2, 2019, for a stratigraphic test well in early 2020, a necessary step toward a North Dakota CO2 Storage Facility Permit (SFP) for the RTE CCS effort. Outcomes include 1) validating the Broom Creek Formation as a regional target for CCS, 2) determining the full carbon life cycle of an industrial fuel production facility with CCS, 3) developing a field implementation plan (FIP) for small-scale CCS, and 4) determining the validity and pathway for using CCS to meet low-carbon fuel (LCF) standards. The technical team included the EERC, RTE, Trimeric Corporation, Schlumberger Carbon Services, and Computer Modelling Group (CMG). Findings from activities conducted November 2016 – May 2020 are summarized as follows. Several key steps have been accomplished toward validating the Broom Creek Formation as a CO2 injection and storage target at the RTE CCS site, including verification of the presence and structure of sandstone layers that may comprise the potential CO2 storage reservoir and the several thousand feet of overlying confining zone. Work included site characterization using existing data, interpretation of seismic data within the study area, and geologic modeling simulation of CO2 injection. Interpreted results estimate 3000 feet of confining zone between the Broom Creek Formation (storage target) and the lowermost underground source of drinking water (e.g., the Fox Hills Formation). The thickness of the Broom Creek injection target varies 230–420 ft within the survey area. Results were used to inform the location of a stratigraphic test well and associated characterization test program. No impediments were identified within the targeted CO2 storage complex that would prevent the project from moving forward. A stratigraphic test well is the next step to validate these results and to acquire remaining data necessary to develop a North Dakota CO2 SFP application. The EERC generated full carbon life cycle estimates for CCS integration with the RTE ethanol facility. Results indicated that an average 40% reduction in CO2 emissions is possible through CCS implementation. Approximately half of the carbon in the overall life cycle for a dry mill ethanol plant is generated through the fermentation process and emitted to the atmosphere; this is the CO2 stream targeted for CCS. The remaining carbon is attributed to corn feedstock farming (diesel, fertilizer), energy for fuel processing (natural gas, electricity), and transportation (diesel) of the fuel product. Life cycle carbon estimates are also affected by the anticipated energy consumption of a potential capture facility, which depend on the type of CO2 product generated. For example, a 30%–40% net CO2 emission reduction is estimated if a liquefied CO2 facility were incorporated compared to a 40%–50% net CO2 reduction if a supercritical “injection-grade” CO2 product is generated; i.e., more energy is required to further refine the CO2 stream, affecting the full carbon life cycle estimates. A CCS FIP was developed and initiated at the RTE CCS site, resulting in the development of several guidance documents: a CO2 Capture Process Design Package, a North Dakota CO2 geologic Storage Permits Template, and a Public Outreach Package for CCS in North Dakota. General FIP components include CO2 capture system, pipeline and well designs; monitoring, verification, and accounting (MVA) plans; geologic characterization and testing programs; and permitting and outreach plans. Vendor bids were also acquired for the CO2 liquefaction facility. Near-surface characterization (groundwater and soil gas sampling) and geologic characterization (seismic survey) were initiated to inform development of a UIC Class VI-compliant MVA plan compliant with a North Dakota CO2 SFP. Designs (well and geologic testing) were completed for a stratigraphic test well compliant with a North Dakota CO2 SFP. In addition, the outreach plan was executed, including community open houses, meetings with city/county/state officials, and development of public materials. Although other entities continued to mature incentive programs in 2019–2020, California and the Internal Revenue Service (IRS) currently provide the most advanced economic opportunities for CCS integrated with fuel production. The California Low-Carbon Fuel Standard (LCFS) adopted a CCS Protocol in January 2019, allowing submittal of a design-based pathway (DBP) application for an approved temporary (not certified) carbon intensity value for a fully engineered facility. An ethanol–CCS DBP application to the California LCFS Program (officially approved February 28, 2020) was developed to show that the RTE CCS effort meets LCFS requirements. The approved DBP provides confidence to advance the project and supports potential investments. Other entities continue to mature incentive programs. The IRS issued guidance in February 2020 that addresses the definition of beginning of construction and revenue procedure on partnerships for the Enhancement of Carbon Dioxide Sequestration Credit (a.k.a. Section 45Q) CCS tax credit program; the IRS anticipates issuing further guidance on issues such as secure geologic storage, utilization qualifications, and recapture of claimed credits. Maturing incentive programs coupled with workable permitting regulations provide confidence to advance CCS projects in North Dakota and support financial investment to proceed with designing, constructing, and implementing CCS projects at small-scale fuel production facilities. The largest hurdles for CCS implementation at small-scale industrial systems are often business/economic-related (i.e., not technical). Market uncertainty already exists for agriculture-based alternative fuels such as corn ethanol, for which production has increased by ~33%, and prices have correspondingly lowered since 2015. Passing the Section 45Q tax credit program improves economic feasibility for CCS but may require external investors for a small business to achieve maximum benefits. Public–private partnerships with NDIC and DOE have resulted in foundational technical and regulatory knowledge, growing stakeholder confidence, and a pathway to implementation that enables similar industrial CCS projects in the region to advance. This subtask was funded through the EERC–DOE Joint Program on Research and Development for Fossil Energy-Related Resources Cooperative Agreement No. DE-FE0024233. Nonfederal funding was provided by NDIC and RTE. The authors would also like to thank CMG, ESRI, IHS, Neuralog, and Schlumberger for allowing the use of their software packages in support of this work.

42 ENGINEERING↗

DOE OSTI2020

Improved Performance of Cu(InGa)(SeS) 2 PV Modules Using the Reaction of Metal Precursors. Final Report

This project “Improved Performance of Cu(InGa)(SeS) 2 PV Modules using the Reaction of Metal Precursors” was a partnership led by the Institute of Energy Conversion (IEC) at the University of Delaware with Columbia University and the Molecular Foundry at the Lawrence Berkeley National Laboratory. The aim was to develop pathways to improve Cu(InGa)(SeS) 2 (CIGSS) thin film photovoltaic modules using processes compatible with low manufacturing cost. The CIGSS approach investigated was a two-step process including deposition of metal precursor films following by reaction in hydride gases utilizing IEC’s novel reactor. The process was similar to that under commercial development by the project’s industry partner Stion. When Stion went out of business mid-project the focus changed to a rapid thermal process considered more commercially viable. Approaches to improve the performance of solar cells using the reacted films focused on two material innovations. First, the overall Ga content was increased to increase the operating voltage, which is desirable for scale-up to commercial modules. Second, the processing and performance advantages arising from Ag alloying were investigated. Advanced characterization guided process and material development including control of relative composition gradients. Research on the formation of Cu-Ga-In metal precursors utilized sputtering deposition which is normally used in commercial applications. The work resulted in processes for deposition of precursor stacks with increased relative Ga content and effects of deposition parameters on morphology and phase composition were established. It was shown that the metal precursor films have comparable phase composition and morphology so subsequent reaction follows from the same starting point. The addition of Ag to the metal precursors gave more uniform morphology and improved adhesion of reacted films which enable higher reaction temperature for faster processing. A novel outcome was the discovery of a previously undocumented material phase in sputter-deposited and evaporated Ag-Cu-In-Ga thin films. Hydride gas reaction processes including time-temperature-concentration profiles were developed for different precursor compositions. This enables control of composition profiles to engineer through-film gradients for solar cell optimization with characterization and simulations used to correlate measured film composition profiles to measurements of devices. In particular, the gradient of sulfur at the front of the CIGSS film was found to be critical. The simulations guided process development leading to improved reproducibility of devices improved performance with higher Ga content and higher voltage. With Ag-alloyed precursors, the reaction pathways leading were determined. A significant finding was that Ag-alloying increases the reaction rate to completely convert precursor films to the final chalcopyrite which could enable reduced reaction time to benefit manufacturability. To maintain potential commercial viability, the process under investigation was refocused to a rapid thermal process that could potentially be incorporated into an in-line process for manufacturing. Precursors with different composition were capped with an extra selenium layer and reacted in hydrogen sulfide 5-15 minutes, compared to typically 2 hours in the previous multi-step batch process. Critical RTP parameters were identified to control the reaction. Further optimization would be needed for high efficiency solar cells but pathways to high quality devices with further optimization and improved heating uniformity were developed. The project also developed new optoelectronic characterization approaches with a focus on development and application of spatial- and time-resolved photoluminescence and a custom mapping photoluminescence microscope built. It was shown how critical electronic transport properties strongly depend on the chemical composition of the material and that a wide range of samples show inhomogeneity on a length scale larger than the grains in the films. Additionally, two-photon excitation capability was developed to distinguish bulk vs surface losses. The project advances the state-of-the -art for precursor reaction processes in several ways that could impact manufacturing. This includes validation of approaches to increase voltage and establishment of model-guided control to form optimal composition profiles. The application of process control approaches with knowledge of phase formation and reaction pathways can be critically valuable in designing a large-scale process.

14 SOLAR ENERGY↗

DOE OSTI2025

The joys and jitters of high‐temperature calorimetry

Abstract High‐temperature calorimetry (HTC) originated in the 20th century as a niche method to enable measurements not easily accomplished with acid solution calorimetry, combustion calorimetry, vapor pressure, or EMF methods. Over time, HTC has evolved into a versatile approach to accurately quantify formation, phase transition, surface and interfacial enthalpies of a wide range of materials including minerals and refractory inorganic compounds. This evolution has been the result of numerous adjustments to experimental setups and procedures, followed by rigorous testing. The commercial availability and the scientific success of this technique have led to an increase in the number of laboratories applying HTC. However, the knowledge acquired by researchers over the past 70 years is scattered throughout the literature or only available as laboratory internal documentation and personal experience. This publication is a collaborative effort among several leading HTC laboratories to summarize and unify current state‐of‐the‐art HTC techniques and procedures. The text starts by summarizing various HT techniques that are commonly used for readers with an interest in HTC in general. It is then directed toward HTC users and includes a brief section on data evaluation procedures as well as a comprehensive compilation of reference data utilizing molten sodium molybdate and lead borate solvents. Finally, for experienced HTC users, an in‐depth discussion of some common difficulties and a discussion of uncertainties are presented.

Scharrer, Manuel [Navrotsky Eyring Center for Mate↗

DOE OSTI2023

Gas-Phase Composition as a Predictive Metric for Calendar Life Behavior of Next-Generation Silicon Anodes

The expansion of renewable technologies and electrification of the transportation sector is driving increased demand for next-generation battery materials that provide higher power and energy density with superior cycling and calendar life stability. Silicon (Si) has a theoretical capacity nearly 10x that of graphite, and is therefore a promising anode material candidate to meet these rigorous performance demands. While leading Si anode battery demonstrations are approaching target metrics for cycle life, a series of complex and interrelated modes of reactivity lead to reduced calendar life and therefore challenge practical adoption of these materials. Deconvoluting the degradation processes that impact Si calendar life is critical to informing the rational and accelerated design of improved Si materials. In the present work, we employ novel sampling techniques and GC-MS-FID characterization to measure gas-phase composition during initial Si cycling, which we tie to selective mechanisms of Si passivation. We utilize a tiered analysis approach to identify and quantify the gas-phase reaction products associated with three advanced Si material candidates under practical operating conditions. Ex situ analysis of Si powders (pure chemical reactivity) is coupled with nondestructive in situ sampling of Si electrodes in a practical pouch-cell format (coupled chemical and electrochemical reactivity). We link the observed gas-phase species evolution to electrochemical behavior and measured calendar life of the three Si materials. Further, we evaluate the voltage-resolved evolution of gas-phase species for one such Si nanomaterial, where nonmonotonic gas generation implies competition between passivating reaction pathways. The measured gas-phase compositional data serves as a critical input for our advanced electrochemical SEI models to identify favorable vs unfavorable reaction pathways to stabilize Si. In addition to bolstering a fundamental understanding of Si reactivity, the present approach informs specific and quantifiable gas-phase metrics tied to calendar life improvements in Si, which can streamline and accelerate the process of next-generation material development.

DIRECT ENERGY CONVERSION,ENERGY STORAGE↗

DOE OSTI2020

Contaminant Migration Modeling to Support the In Situ Decommissioning of Hardened Nuclear Facilities - 20215

The decommissioning of hardened nuclear facilities provides a unique challenge in balancing current worker dose with exposure to future receptors and media. In situ decommissioning (ISD) is a cost-effective and safe option for the closure of such facilities but requires a detailed understanding of the threat that radioactive and hazardous constituents remaining in the facilities pose to groundwater and surrounding surface water. The Savannah River Site (SRS) extensively employs contaminant migration models within the decommissioning process to develop site-specific removal, grouting, and monitoring strategies in support of safe and effective final end states of nuclear facilities. This work discusses the use of contaminant migration modeling in the ISD process at SRS, including specific examples from the closure of P-Reactor and R-Reactor, Building 235-F, F-Canyon and F/H Laboratory Complex. Migration models developed during the closure of P-Reactor and R-Reactor were divided into four source areas: the reactor vessel, the process area, the disassembly basin, and the purification wing. Each source area was assigned a specific inventory and migration pathway and was then subject to varying hypothetical removal, capping, and grouting schemes. Modeling indicated that groundwater Maximum Concentration Limits (MCLs) might be exceeded if no action was taken for eleven and ten constituents of concern (COCs) at P-Reactor and R-Reactor, respectively. These exceedances could occur in as few as 200 to 500 years. Alternatively, the migration modeling demonstrated that the selected ISD actions reduced contaminant mobility which allowed for significant radioactive decay and resulted in fewer predicted exceedances of groundwater MCLs (five COCs for P-Reactor; eight COCs for R-Reactor). In response to the modeling results for P-Reactor and R-Reactor, effectiveness monitoring programs were developed to target contaminants, specific to each reactor, that may migrate to groundwater. Contaminant migration modeling also revealed that roof collapse was a large factor in the release of COCs to the environment, giving rise to roof improvements, and an inspection and vegetation control program to ensure roof stability over time. Contaminant migration modeling is also aiding in the closure planning for hardened facilities in F Area. Building 235-F housed the Actinide Billet Line, which produced Np-237 billets for irradiation in SRS reactors, and the Plutonium Fuel Form (PuFF) facility that produced Pu-238 heat sources for the space program. As a result of these missions, areas within Building 235-F contain considerable residual amounts of both Pu-238 and Np-237. Contaminant migration modeling of Building 235-F was originally performed in 2012 to identify the feasibility of ISD and the amount of radioactive material removal required to prevent the exceedance of groundwater MCLs. The original model indicated that a 60% reduction in the PuFF facility Pu-238 inventory could keep groundwater concentrations below standards, while Np-237 did not pose a threat to groundwater. However, updates to the model with an emphasis on source impact pathways revealed that, due to the orientation of the source areas relative to groundwater flow, no amount of reasonable removal of Pu-238 would keep groundwater concentrations below MCLs and that Np-237 could be a large contributor to localized MCL exceedances. With this insight, the refined 2019 model is being used to assist in the development of grouting plans specific to each facility source area, where bentonite may be utilized to slow the migration of Pu-238 and its daughter products from the PuFF facility and a reducing grout may decrease Np-237 transport by ensuring the nuclide remains in the less mobile +IV oxidation state. The beginning phases of contaminant migration modeling are underway for F-Canyon and associated facilities using lessons learned from the Reactors and Building 235-F. A contaminant migration pathway, similar to the pathway used for the reactor vessels, is being developed for the hot and warm canyons. The F-Canyon inventories are being spatially refined to identify specific and localized source zones, comparable to Building 235-F, that may impact groundwater. Contaminant migration modeling provides vital input within the ISD process, from facility investigation to post closure effectiveness monitoring, making it a valuable tool in the development of safe and effective end states for hardened nuclear facilities at SRS. (authors)

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DOE OSTI2023

COMPUTATIONAL MODELING OF IGNITION AND PREMIXED FLAME PROPAGATION INITIATED BY A PRE-CHAMBER TURBULENT JET

Addressing the pressing need for reduced carbon emissions, Turbulent Jet Ignition (TJI) emerges as a promising technology for ultra-lean combustion, offering enhanced thermal efficiencies and minimized cyclic variability in spark-ignited engines. To facilitate rapid testing and integration of this technology, a robust computational modeling framework is crucial. This study delves into the predictive capabilities of computational models for main-chamber ignition and premixed flame propagation using a single-cycle TJI rig measured by Biswas et al. (Applied Thermal Engineering, vol 106, 2016). Employing an open-source compressible flow simulation solver with Large Eddy Simulation (LES) for turbulence modeling, the investigation integrates the conventional Laminar Finite Rate Chemistry (LFRC) model alongside the transported Probability Density Method (PDF) for turbulence-chemistry interaction. A fully-consistent Eulerian Monte-Carlo Fields (EMCF) method is utilized to approximate the transported PDF, while Interaction by Exchange with Mean is employed to close micro-mixing terms in stochastic differential equations. A reduced chemical reaction mechanism with 21 species and 84 reactions (DRM-19) is used for solving chemical kinetics, and a double Gaussian energy deposition model is used to approximate the spark ignition in the pre-chamber. An unstructured O-grid mesh with 0.3 million cells in the prechamber and 1 million cells in the main chamber is employed. Results are divided into two phases: pre-chamber initialization and full TJI simulations. Validation of the predicted pre-chamber flame propagation and the lean ignition in the main-chamber is carried out by using available experimental data. Under quiescent conditions, both the LFRC and transported PDF methods largely underestimate the flame speed and subsequent pressure growth in the pre-chamber. A linear momentum forcing technique is applied to investigate the impact of initial turbulence in the pre-chamber, demonstrating a notable influence on flame propagation. Fine-tuning of the forcing coefficient reproduces the sudden pressure growth observed in the experiment. The experimentally validated pre-chamber simulation serves as the initial condition for the full TJI simulations. It is found that the LFRC model fails to predict lean-ignition in the main-chamber, resulting in a misfiring event. Incorporation of turbulence-chemistry interaction using the transported PDF method substantially improves the prediction of the ignition event in the main-chamber, achieving fair qualitative agreement and quantitative validation of combustion parameters within ±10% of the reported experimental data. The rich simulation results consisting of a full set of statistical description of the thermo-chemical states enable us to gain deep insights into the ignition mechanisms in the main chamber, which is limited when done experimentally. A novel dual ignition phenomenon is revealed in the TJI rig for the first time. Initially, a primary ignition kernel is formed at a downstream location which eventually detaches from the main jet. As the jet momentum decreases, a secondary ignition event follows, this time at a more upstream location which eventually combines with the primary ignition kernel to form a single connected flame front. Investigation of these ignition sequences in chemical composition space reveal distinct differences between the two. The primary ignition event in the main-chamber is followed by a large concentration of active radicals from the pre-chamber jet, accelerating the chain-branching steps, characterizing what has been referred to as flame ignition. In contrast, the secondary ignition occurs in the absence of active radicals in the pre-chamber jet, hence characterized as jet ignition. Further analysis of the effect of pre-chamber jet characteristics on lean ignition in the main-chamber is conducted by setting up cases with different initial pressure ratios (por) between the two chambers, a non-dimensional parameter, ranging from 1.2 to 3.2. As the initial pressure ratio increases, jet momentum increases, with dual ignition observed in cases above por= 2.2. Case with por= 3.2 lead to misfiring. The effect of ignition sequence on global combustion characteristics of TJI is analyzed. Dual ignition events lead to non-monotonicity in combustion characteristics such as global reaction progress variable, flame penetration, and global heat release rate. In dual ignition events, although the rate of fuel consumption and global heat release rate is initially lower, the secondary ignition leads to a sudden increase in flame surface area, resulting in a sudden jump and promoting the overall performance of the TJI system.

42 ENGINEERING↗

DOE OSTI2024

Liquid Piston with Spray Cooling Near-Isothermal Compressor

The goal of this project was to prototype and characterize the performance of a liquid-piston spray-cooled gas compressor. The working principle of the compressor enables optimized high-efficiency operation over a very wide range of operating conditions, unlike conventional compressors that are optimized for a narrow range of operating conditions. The compressor technology is suitable for many applications, such as gas pipeline transport, gas storage, and commercial and residential heat pumps. Both physical testing and computational fluid dynamics (CFD) modeling of the processes using the Oak Ridge National Laboratory high-performance computing center were completed. The experimental and CFD studies focused on a near-isothermal liquid-piston compressor (LPC) that uses propylene glycol to compress CO 2 . The first prototype demonstrated isothermal operation during several sequentially executed cycles of CO 2 compression and raised the temperature of the compressed CO 2 by only 2 K, compared with approximately 6 K when the gas was compressed non-isothermally. Isothermal operation was demonstrated at CO 2 flow rates of up to 2 L/min. The second prototype was designed with two compression chambers to allow continuous flow of high-pressure CO 2 . However, the design of the valve train to direct flow between the compression chambers was not sufficient to allow demonstration of CO 2 compression. Numerical simulations of the LPC in which the compression chamber was filled with propylene glycol injected from the bottom inlet were performed using large eddy simulation (LES) with the wall-adapting local eddy-viscosity subgrid-scale model coupled with the multiphase volume of fluid (VOF) model to simulate the transient interface between gas and liquid and to capture the heat and mass transfers within the compression chamber. In this effort, the effects of boundary conditions applied to the LES-VOF calculations (i.e., no wall, an adiabatic wall, and a wall with a heat flux subscribed) on the overall pressure and temperature of the CO 2 gas as well as the transient evolution of flow and heat transfer within the compression chamber were investigated and are discussed in this report. The LES calculation with no wall showed no dynamical flow patterns, and the volume-averaged temperature of CO 2 increased from 305 to 392.7 K, whereas LES calculations with a constant wall temperature or a wall heat flux had similar increases of CO 2 temperatures. The results of the LES simulation using a wall heat flux showed different stages in the compression process and revealed dynamical formation and interaction of CO 2 gas layers and circulation flow patterns within the chamber that contributed to the overall heat transfer between the solid wall, gas, and liquid surface in the compressor. Though an industrial partnership for commercializing the compressor was not secured, the technology was attractive for an industrial partner to use in two research proposals in response to US Department of Energy funding opportunity announcements.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2025

Fostering a Guiding Multiscale Model for the Development of Advanced MgB 2 Hydrogen Storage Materials (Final Technical Report)

Project Goal and Objective. The demand for energy and for an upgraded energy infrastructure has steadily grown, as have the needs for energy independence and alternatives to our reliance on petroleum. Hydrogen is considered the most viable fuels for wide-scale implementation in the near future as it is less-polluting, non-toxic, and has more stored energy than petroleum. It is envisioned that hydrogen can eventually become the prime energy carrier, integrating the transportation, grid, and chemical sectors in a way that improves resiliency, diversifies feedstocks, and affords new economic opportunities. A key remaining challenge is the development materials with enhanced gravimetric and volumetric hydrogen storage capacities that offer a higher performance than compressed gas. These materials would eliminate the need for large-scale compression, thereby dramatically reducing the footprint and cost of gas storage. The high gravimetric and volumetric hydrogen capacities of complex hydrides has prompted an intensive investigation of the potential of this class of materials as hydrogen storage media over the past 25 years. Among the many complex hydrides that have been explored, magnesium borohydride, Mg(BH 4 ) 2 , has been found to possess the best combination of practical thermodynamic properties. These include a gravimetric H 2 density of 14.9 wt% H 2 and thermodynamics for the dehydrogenation of Mg(BH 4 ) 2 to MgB 2 (equation 1) (ΔH° = 39 kJ/mol H 2 , ΔS = 112 J/K mol H 2 ) which lie in the narrow window required Mg(BH 4 ) 2 $\Leftrightarrow$ MgB 2 + 4 H 2 (1) for reversibility under moderate pressure and temperature. However, overcoming the extremely slow kinetics of the reversible release of hydrogen by this material in the solid state is a daunting challenge. At temperatures greater than 400 °C, the borohydride releases up to 14 wt% hydrogen giving MgB 2 . We discovered that the direct re-hydrogenation of MgB 2 to Mg(BH 4 ) 2 can be accomplished under 950 bar H 2 at 400 °C. While this demonstrated that complete reversibility can be achieved, the conditions employed are far too extreme for commercial hydrogen storage applications. More recently, we found through US DOE funded research projects (EERE HyMARC and HySCOR), that hydrogen cycling, can be accomplish at much milder conditions upon modification of the borohydride or boride. Guided by these discoveries these discoveries, the objective of this research project was to obtain key information that will enable the development of a model of reversible hydrogenation of MgB 2 to Mg(BH 4 ) 2 . The ultimate goal of our efforts is to attain a model of this transformation that can be utilized to accelerate development further advanced materials. This project directly follows on discoveries that were made over the course of a US DOE, EERE HyMARC project that was focused on improvement of the hydrogen cycling kinetics of modified MgB 2 . We found that that mechanical milling with graphene results the desired, pronounced kinetic enhancement. The dramatic lowering of the conditions required for the hydrogenation of MgB 2 is a significant step towards overcoming its chemical inertness allowing its development as a practical onboard hydrogen storage material. However, the exact nature of the modification(s) of MgB 2 that is responsible for its activation towards hydrogenation is completely unknown. This situation is not unique, as efforts to develop hydrogen storage materials typically have a narrow focus rather than a comprehensive approach that takes atomic level bonding and structure; molecular dynamics; long range, nano- and mesoscale-structure and their interconnection all into account. The goal of this project was the development of a comprehensive, multi-scale computational model of reversible hydrogenation of MgB 2 to Mg(BH 4 ) 2 that can be utilized for development of higher performance versions of the modified material. Development of the model requires determination of: 1) the bulk, nano-scale, and meso-scale structural changes occurring at elevated pressure following mechano-chemical modification of MgB 2 ; 2) the reaction pathway of the reversible hydrogenation of MgB 2 to Mg(BH 4 ) 2 ; 3) the effect of elevated pressure and mechano-chemical modification on the chemical reaction pathways; 4) the interactions at solid-gas interfaces; and particle surfaces; and 5) the kinetics and thermodynamic parameters associated with each step of the hydrogenation reaction pathway. This investigation required advanced techniques as preliminary, standard XRD, 11 B NMR, and FTIR analysis showed no signs of material modification. In order to gain this level of understanding of modified MgB 2 , required the teaming of a diverse group of experts and state-of-the art experimental capabilities at the University of Hawaii at Manoa (UHM) and collaborating National Laboratories: Craig Jensen , Department of Chemistry (PI and Project Director), solid state, solution, and high pressure NMR spectroscopy; solid-state synthesis; and high pressure hydrogenation (collaboration with SNL); Godwin Severa , Hawaii Natural Energy Institute (co-PI) calorimetry; infrared and Raman spectroscopy (collaboration with NREL); Dera , high pressure X-ray diffraction including in situ experiments (collaboration with ANL); Hope Ishii , Hawaii Institute of Geophysics electron microscopy investigations (collaboration with LBNL); and Joe Brown , Mechanical Engineering , material electronic structure and electric field effects.

08 HYDROGEN↗

DOE OSTI2020

Development of the Mobile Systems for Conditioning of Disused Sealed Radioactive Sources in Serbia - 20105

Sealed radioactive sources (SRS) are being used worldwide in the field of medicine, agriculture, industry and research. They can be found in mobile as well as stationary devices. SRS contains radioactive material that is (a) permanently sealed in a capsule or (b) closely bounded and in a solid form. The capsule or material of an SRS should be strong enough to maintain leak tightness under the conditions of use and purpose for which the source was designed, also in case of accidents. In this case only emitted radiation is utilized. Firstly, the hazard from external radiation has to be considered, but the possibility of contamination due to fracture of the capsule should not be disregarded. The radioactive sources are composed of the radiating isotope contained in the filling medium, the single or double isotope holder that partially or totally surrounds the filling medium, the outer cover that contains the parts mentioned above and the capsule closed airtightly by welding or using some other method. The capsule must be tested for leakage periodically. If the SRS is no longer needed (e.g. replaced by a different technique) or it becomes useless for the intended application (e.g. the activity becomes too weak, the equipment containing the source works poorly or becomes obsolete, the source is damaged or leaking) it is considered disused. Disused sealed radioactive sources (DSRS) are typically conditioned and disposed if a facility is available. If the disposal option is not available, conditioned DSRS should be stored under proper conditions. In some cases, the radionuclide(s) in DSRS can be recovered/recycled or the DSRS can be repurposed for other applications. Conditioning of DSRS ensures containment of the radioactive material, provides confinement for leaking sources, provides sufficient radiation shielding, reduces storage/disposal volume by allowing consolidation of multiple sources into a single storage/disposal container, facilitates transport operations and contributes to safety and security as well. Typically, conditioning technologies are deployed either as permanently installed stationary systems in centralized or mobile on-site waste processing facilities, or in a mobile configuration. Centralized stationary facilities provide a single processing location for multiple users that requires transport of the waste to the facility. On the other hand, mobile systems may be provided for the selection and application of the optimum technology for a specific waste stream (such as DSRS) by bringing the process to the point where the waste is generated. In addition, mobile systems could offer additional flexibility by sharing equipment among multiple waste generating sites for processing campaigns that vary in duration, from very short periods to several years. The term 'mobile processing system' refers to any radioactive waste processing system or component which is designed to be transportable and which is not considered permanently installed. Two mobile system for conditioning of disused sealed radioactive sources are developed in the Public Company Nuclear Facilities of Serbia. Development of these mobile systems was supported by SRB9005 national project via Technical Cooperation of the IAEA. The first mobile system, built inside the 20 feet ISO container, will be used for conditioning of DSRS category 3 to 5. The second mobile system, built inside the 7 m long vehicle (Iveco Daily Van), will be used for dismantling of ionizing smoke detectors mostly with Am-241 sources. Designs of the mobile systems were defined in cooperation with two companies from Belgium (Belgoprocess and Leniko) and a Croatian company Ekoteh as well as with the support of the IAEA experts. The generic safety assessment and operational procedures for the mobile systems are developed. Based on safety assessment the acceptance criteria and operational limits and conditions are established. Operational procedures include: (a) equipment and material requirements, (b) assembling procedure of the mobile unit, (c) procedure for acceptance of devices for dismantling and conditioning, (d) dismantling procedure for devices to recover the DSRS, (e) characterization of DSRS, (f) encapsulation procedure of DSRS, (g) disassembling procedure of the mobile unit, and (h) keeping records, identification and traceability. In addition, radiation safety, health safety, security and emergency preparedness plans are prepared. The generic safety assessment and operational procedures could be updated with site specific requirements, DSRS inventory, and different needs for future customers. Developed mobile systems could be used in all situations when it is feasible to perform conditioning of DSRS on the spot in the county and worldwide. Development of these mobile units was just the first step to create the Reference Center for Radioactive Waste Treatment and Disused Radioactive Sources Conditioning for Small Facilities which can become a regional training center in the future, and/or as a tool for comprehensive national search and secure programmes. In the next phases development of e-learning platforms and blended learning packages as well as application for the IAEA Qualified Technical Centre (QTC) for the management of DSRS is foreseen. (authors)

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