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Woods, Michael Ellis

Publications and source records attributed to Woods, Michael Ellis.

12 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Corrosion Testing Of Additively Manufactured Stainless Steel 316H In Molten Salt Environments

The development of a new ASTM standard for evaluating the corrosion resistance of additive manufactured (AM) stainless steel (SS) 316H in chloride molten salts is critical for the use of these materials in extreme environments such as molten salt reactors (MSRs). This report pertains to a work package of the Advaned Materials and Manufacturing Technologies (AMMT) developing a systematic methodology to link changes in AM fabrication parameters, namely surface finishing, porosity, microstructure, and chemical heterogeneity, to corrosion performance in NaCl-MgCl2 salt, a proposed secondary coolant for MSRs. During Fiscal Year 2024, Idaho National Laboratory investigators in the AMMT program, utilized SS316H bars, fabricated with laser bed powder fusion at Los Alamos National Laboratory, to establish and optimize the workflow for evaluating these process-to-performance relationships. Standard practices for specimen preparation were established using these specimens, with particular focus on descaling and sectioning methods that align with ASTM guidelines. A comprehensive experimental design for static corrosion testing was developed, with pre- and post-exposure analysis utilizing optical microscopy and scanning electron microscopy. So far standard descaling techniques were optimized, one static corrosion test was conducted on the LANL AM SS316H specimens, and pre- and post-corrosion practices were established. In addition, the work package yielded a review paper on corrosion testing gaps for AM materials in nuclear applications and submitted a proposal for a rapid-turnaround experiment to the Nuclear Science User Facilities Program to investigate the combined effects of proton irradiation and corrosion on AM SS316H. This work package establishes a foundation for evaluating processing-to-performance relationships for AM SS316H in harsh conditions, contributing to the safe and efficient design of components for next-generation nuclear reactors. The creation of a standardized methodology and the generation of relevant publications and future research pathways represent significant strides towards integrating AM materials into critical applications where corrosion resistance is paramount.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Natura Resources Molten Salt Research Reactor (MSRR) Fuel Workshop: Summary Report

Idaho National Laboratory (INL) hosted the Natura Resources team in Idaho Falls for a 3-day fuel workshop, July 16-18, 2024. The purpose of this workshop was to understand Natura’s fuel requirements, determine the feasibility of producing that fuel at INL, and define the scope of work that would enable fueled operation of the Natura MSR-1 being deployed at Abilene Christian University (ACU).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Elucidating the Transition of 3D Morphological Evolution of Binary Alloys in Molten Salts with Metal Ion Additives

Molten salts serve as effective high-temperature heat transfer fluids and thermal storage media used in a wide range of energy generation and storage facilities, including concentrated solar power plants, molten salt reactors and high-temperature batteries. However, at the salt–metal interfaces, a complex interplay of charge-transfer reactions involving various metal ions, generated either as fission products or through corrosion of structural materials, takes place. Simultaneously, there is a mass transport of ions or atoms within the molten salt and the parent alloys. The precise physical and chemical mechanisms leading to the diverse morphological changes in these materials remain unclear. Here, to address this knowledge gap, this work employed a combination of synchrotron X-ray nanotomography and electron microscopy to study the morphological and chemical evolution of Ni-20Cr in molten KCl-MgCl 2 , while considering the influence of metal ions (Ni 2+ , Ce 3+ , and Eu 3+ ) and variations in salt composition. Our research suggests that the interplay between interfacial diffusivity and reactivity determines the morphological evolution. The summary of the associated mass transport and reaction processes presented in this work is a step forward toward achieving a fundamental comprehension of the interactions between molten salts and alloys. Overall, the findings offer valuable insights for predicting the diverse chemical and structural alterations experienced by alloys in molten salt environments, thus aiding in the development of protective strategies for future applications involving molten salts.

36 - MATERIALS SCIENCE↗
DOE OSTI2024

Surface Preparation of Additively Manufactured 316H Stainless Steel for Molten Salt Applications

Additive manufacturing (AM) has the potential to revolutionize the manufacturing process and speed up deployment of advance nuclear reactors. However, more information is needed on preparing AM materials for extreme reactor environments to qualify AM materials for nuclear applications. This project studies the surface preparation of AM 316H stainless steel using acid pickling and reports a successful procedure for descaling heat-treated AM material.

316H Stainless Steel↗
DOE OSTI2024

Radiation-induced transients on solid and molten Li and K iodides

The study, quantification, and monitoring of iodine in nuclear power generation systems have been paramount due to its environmental and health implications. Thorough speciation and transport studies strengthened the development and deployment of water reactors, which are now required for the new generation of Molten Salt Reactors (MSR), where the fuel and coolant are a complex liquid system of suitable halides. The speciation, radiation-induced chemistry, and transport of iodine (I-127, I-129 and I-131) under extreme conditions of temperature and ionizing radiation are among the challenges for the future implementation of MSR’s. In aqueous systems, the triiodide-iodine-iodide (I3--I2-I-) equilibrium is strongly dependent on the conditions of the medium. In molten iodides and chlorides, the triiodide detection (and its disproportionation) poses challenges due to the extreme conditions of temperature and radiation, but studies have shown a dependence on temperature, absorbed dose and salt composition. Through absorption spectroscopy techniques (diffuse reflectance and high-temperature UV-Vis), as well as resonance (Electron Paramagnetic Resonance) it is possible to identify primary transients induced by ionizing radiation trapped in the solid phase (Solid-state radiolysis), and steady-state main absorption components with a fast-acquisition real-time spectroscopy. The presence of heterogeneous phase (colloids), viscosity changes, and gas evolution are among the observed processes. A specific case of study is speciation in the presence of Ni. A corrosion product with magnetic properties due to unpaired electrons in its electronic structure. Ferromagnetic materials are monitored in solidified salts to identify aggregation and phase separation. Comparative studies of eutectic mixtures of LiI-KI and LiCl-KCl with known addition of dopants will be presented, with a perspective of radiation chemistry and its possible implications in complex systems.

36 - MATERIALS SCIENCE↗
DOE OSTI2024

Kinetics of Radiation-induced Cr( II ) and Cr( III ) Redox Chemistry in Molten LiCl-KCl Eutectic

Chromium (Cr) is a frequent constituent of the metal alloys proposed for molten salt nuclear reactor (MSR) applications, and is typically the least noble metal ion present. Consequently, chromium is preferentially corroded into molten salt solutions. Here, the redox poise and redox cycling of chromium ions in the salt can greatly influence its corrosivity towards structural alloys, ultimately impacting the longevity of MSR systems. Radiation-induced chemistry is expected to play a significant role in determining the chromium oxidation state distribution during MSR operations. In the present research, electron pulse radiolysis techniques were employed to characterize the reactivity of Cr(II) and Cr(III) ions with primary radiolysis products in molten lithium chloride–potassium chloride (LiCl–KCl) eutectic over a temperature range of 400–600 °C. Both chromium oxidation states were found to rapidly react with the primary products of molten chloride salt radiolysis, i.e., the solvated electron (e S - ) and the dichlorine radical anion (Cl 2 ˙ - ). For reactions with the e S - , second-order rate coefficients (k) of k = (4.1 ± 0.2) and (6.1 ± 0.3) × 10 10 M -1 s -1 at 400 °C for Cr(II) and Cr(III), respectively, were determined. Temperature-dependent measurements allowed for the derivation of activation parameters for electron capture by Cr(II) and Cr(III). Both chromium ions also react with Cl 2 ˙ - , k = (7.2 ± 0.3) and (1.4 ± 0.1) × 10 9 M -1 s -1 at 400 °C for Cr(II) and Cr(III), respectively.

37 - INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL C↗
DOE OSTI2023

Milestone 1.2.15: Feasibility of In Situ Accelerated Aluminum Coupon Radiolysis by Synchrotron X-Rays

Extended dry storage of aluminum-clad spent nuclear fuel (ASNF) requires an assessment of the radiolytic generation of molecular hydrogen gas (H2) from the ASNF’s corrosion layers. H2 accumulation can potentially lead to storage canister embrittlement/rupture and the accumulation of flammable gas mixtures in accident scenarios. To date, computational models have been developed for the prediction of radiolytic H2 generation from samples exposed to lower absorbed dose regimes (up to ~3 MGy). However, greater accuracy is needed for higher absorbed doses (> 25 MGy) where the concentration of H2 ultimately reaches a steady-state. Data in this area is limited due to the amount of time taken (months) to accumulate such high gamma doses. Furthermore, a recent study observed radiation-induced damage to the surface of pre-corroded aluminum alloy coupons at high absorbed gamma doses. Despite this observation and its implications, there is currently no computational connection between the radiolytic formation of H2 and changes in the composition and morphology of the cladding’s corrosion layers with absorbed dose. To develop a better understanding of the processes and effects described above, the present study aimed to evaluate the feasibility of leveraging synchrotron x-ray capabilities for coupled accelerated irradiation and in situ surface characterization of ASNF alloys. To that end, National Synchrotron Light Source II (NSLS-II) beamtime was secured and a series of aluminum alloy 1100 (AA1100) wires, prepared under a variety of conditions, were interrogated using ex situ x-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques at Idaho National Laboratory (INL) and ex situ and in situ XRD capabilities at the NSLS-II x-ray powder diffraction (XPD) beamline. Results indicated that performing synchrotron XRD using the available XPD beamline configuration can provide sufficient radiation dose but cannot discern changes in the composition and morphology of sample corrosion layers. Additionally, ex situ XRD and SEM data from Idaho National Laboratory (INL) indicated that the pre-corrosion of AA1100 wires did not generate an appreciably thick corrosion layer, as compared with previous aluminum coupon studies. These thinner surface corrosion layers were not sufficient for detection by both ex situ and in situ synchrotron XRD, specifically under consideration of the NSLS-II XPD beamline’s configuration primarily capturing information from the sample’s bulk material, i.e., aluminum metal. In summary, the use of the NSLS-II XPD beamline for promoting accelerated radiolysis and in situ surface characterization is not appropriate for this program’s goals.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2023

Analysis and Thermal Property Investigations into Ternary Actinide Chloride Salt Systems Containing UCl3 and PuCl3

While regulators, the scientific community, and MSR developers still lack access to literature data on the thermal properties of clean fuel salts, even less information is available on the properties of fuel salts containing impurities. It is essential to understand, benchmark, and predict crucial data on the changes in thermal properties of fuel salt systems due to impurities arising from moisture, corrosion, and reactor operation (i.e., fission products). This research focuses on two actinide fuel salts (1) to investigate a worst-case scenario buildup of actinide fission product in a NaCl-UCl3 eutectic fuel salt and (2) to investigate NaCl-PuCl3 eutectic salt after 1000 hours of operation in a natural circulation flow loop flow to determine if corrosion or atmospheric (moisture/oxygen) products are present. For the first salt, a conservative assumption or worst-case scenario, for fission product buildup in a fuel salt was investigated by adding PuCl3 to eutectic 67 mol% NaCl – 33 mol% UCl3 salt resulting in a ternary salt having a composition of 61 mol% NaCl – 30 mol% UCl3 – 9mol% PuCl3. Addition of PuCl3 to eutectic NaCl-UCl3 resulted in a ternary salt that had a higher melting temperature than either the NaCl-PuCl3 or NaCl-UCl3 binary eutectic mixture. Addition of PuCl3 also resulted in an increase in density which was expected. The second salt was extracted from a micro loop. The composition of the fuel (primary) salt prior to flow loop operations was determined to be 64 mol% NaCl – 36 mol% PuCl3, however, the post-flow loop salt showed increased levels of MgCl2 and NaCl changing the salt composition to 10 mol% MgCl2 – 63mol% NaCl – 26mol% PuCl3) indicating the primary salt interacted with the rinse salt. Analysis of the post flow loop salt detected low concentrations of Al, Ni, Co, Nb, and Zr, most likely corrosion products from the flow loop material of construction. Contamination of the fuel salt (with the rinse salt NaCl-MgCl2) decreased the density by approximately 10% and reduced the onset of melting temperature by 50 °C, from 451 °C to approximately 400 °C. Results from the fission product simulated salt (61 mol% NaCl – 30 mol% UCl3 – 9mol% PuCl3) and the corrosion product salt (10 mol% MgCl2 – 63mol% NaCl – 26mol% PuCl3) will be included in two separate manuscripts for submission to peer-reviewed journals.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

TMS 2023 - Methodology and Density of PuCl3-NaCl Mixtures

The development of molten salt reactors and their associated components demands reliable and accurate thermophysical property data for design and validation. A candidate fuel salt, PuCl3-NaCl (36 mol% PuCl3) has been synthesized and studied at the Idaho National Laboratory. This study has determined the density of PuCl3-NaCl at multiple compositions and temperatures, providing data for validation of modeling efforts and making improvements on the buoyancy method for density measurements of actinide-bearing molten salts.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Radiolytic evaluation of select sulfur chlorides (S 2 Cl 2 and SOCl 2 ) for advanced low temperature chlorination of zirconium-based used nuclear fuel cladding

New sulfur chloride compounds—sulfur monochloride (S 2 Cl 2 ) and thionyl chloride (SOCl 2 )—have been proposed as alternative chlorinating agents for the chemical decladding of zirconium-based used nuclear fuel cladding materials. However, the radiation stability of these compounds has not been thoroughly evaluated, despite envisioned process conditions involving intense, multi-component radiation fields. Knowledge of the radiation chemistry of these sulfur chlorides is essential for the development and optimization of alternative chlorination technologies. To this end, we present preliminary findings on the gamma radiolysis of neat S 2 Cl 2 and SOCl 2 at ambient temperature up to ~ 34 MGy. In this study, Raman spectroscopy and density functional theory calculations were used to identify the Raman-active degradation products from S 2 Cl 2 and SOCl 2 radiolysis. Both sulfur chloride compounds exhibited significant radiation resistance, with respect to changes in the Raman signatures of the parent compounds and the ingrowth of Raman-active degradation products. For S 2 Cl 2 , molecular chlorine (Cl 2 ) was directly identified as the predominant degradation product, which was completely consumed at higher absorbed doses (> 9 MGy). Similarly, the main degradation product from SOCl 2 radiolysis was also Cl 2 , although in this system it continued to grow in with dose over the entire dose range. Further, an “S=O” containing degradation product(s) was also identified as a compliment to Cl 2 . Overall, the perceived radiation resistance of these sulfur chloride compounds makes them suitable for inclusion in a used nuclear fuel chemical decladding process, especially as radiolytically formed Cl 2 can be used to reform the parent compounds, thereby increasing the longevity of the solvents used.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2022

Wetting Properties of Molten Salts

Wettability is a key piece of information in understanding the behavior of molten salts at material interfaces. Wettability is most easily characterized by contact angle which is measurable using the sessile drop method. A modified sessile drop method was used to measure the contact angle of the LiCl-KCl eutectic at varying temperatures on Nickel 200, Hastelloy C276, Glassy Carbon, and MACOR machinable ceramic. The contact angle was used with existing surface temperature data to find the work of adhesion at various temperatures. Finally, problems encountered during the experiment are listed and possible improvements are provided.

36 MATERIALS SCIENCE↗