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At least 613 records · Page 34

Custom Equipment Development for Processing of Surplus Plutonium

The Strategic Laboratory Assessment (SLA), a collaborative team of SRNL and ORNL personnel, has been established to advance the objectives of the Surplus Plutonium Disposition (SPD) Project, by identifying and developing technologies to accelerate disposition, reduce life cycle costs, minimize worker radiation exposure, improve worker safety, and minimize Surplus Plutonium Disposition Program risks. [1] The SLA team has identified can cutting and plutonium (Pu) oxide size reduction as two glovebox processes where technology enhancements would be valuable. The DOESTD-3013 package currently in use for Pu downblending requires cutting two nested cans before the inner convenience can that holds the Pu oxide may be accessed for further processing. A rotary tubing-style cutter is used for opening the 3013 packages within the glovebox. Collet changeouts are required between cutting of the outer and inner cans. The SLA team is currently developing and testing an adjustable-clamp can cutter design that eliminates collet changeouts and allows cutting of the outer and inner can at the same time, resulting in significant reduction of radiological dose and process time, as well as improved ergonomics. To meet the Pu oxide particle size requirement, size reduction of Pu oxide agglomerations must be performed within the process gloveboxes. The SLA team has identified jaw crushing technology as an alternative to the currently employed rotary mill. Jaw crusher advantages include reduced dust within the glovebox, increased batch sizes, and easier integration with other glovebox processes due to the flow-through nature of jaw crushing. Commercially manufactured jaw crushers are either too large and/or too heavy for implementation in the SPD gloveboxes, so the SLA team is developing and testing a custom jaw crusher to meet the needs of the SPD Project.

Krementz, Daniel [Savannah River National Laborato↗

Computationally Accelerated Discovery and Experimental Demonstration of Gd0.5La0.5Co0.5Fe0.5O3 for Solar Thermochemical Hydrogen Production

Solar thermochemical hydrogen (STCH) production is a promising method to generate carbon neutral fuels by splitting water utilizing metal oxide materials and concentrated solar energy. The discovery of materials with enhanced water-splitting performance is critical for STCH to play a major role in the emerging renewable energy portfolio. While perovskite materials have been the focus of many recent efforts, materials screening can be time consuming due to the myriad chemical compositions possible. This can be greatly accelerated through computationally screening materials parameters including oxygen vacancy formation energy, phase stability, and electron effective mass. In this work, the perovskite Gd 0.5 La 0.5 Co 0.5 Fe 0.5 O 3 (GLCF), was computationally determined to be a potential water splitter, and its activity was experimentally demonstrated. During water splitting tests with a thermal reduction temperature of 1,350°C, hydrogen yields of 101 μmol/g and 141 μmol/g were obtained at re-oxidation temperatures of 850 and 1,000°C, respectively, with increasing production observed during subsequent cycles. This is a significant improvement from similar compounds studied before (La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3 and LaFe 0.75 Co 0.25 O 3 ) that suffer from performance degradation with subsequent cycles. Confirmed with high temperature x-ray diffraction (HT-XRD) patterns under inert and oxidizing atmosphere, the GLCF mainly maintained its phase while some decomposition to Gd 2-x La x O 3 was observed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Fundamentals of SrCoO 3-δ Based Oxygen Deficient Perovskites as Cathodes for Solid Oxide Fuel Cells

The local structure and oxygen stoichiometry in oxide systems have a profound impact on oxygen electrocatalysis encountered in metal-air batteries and solid oxide fuel cells (SOFCs). However, this knowledge is often obtained under conditions different from the real working conditions of the material, resulting in misinterpretation and misunderstanding. This PhD dissertation aims to obtain the structure and oxygen-stoichiometry information of a class of perovskite oxides under their real working conditions in solid oxide fuel cells. Several perovskite oxides were selected for the study: Sr 0.9 Y 0.1 CoO 3-δ (SYC10), Sr 0.9 Y 0.3 CoO 3-δ (SYC30), SrCo 0.9 Nb 0.1 O 3-δ (SCN10) and SrCo 0.9 Ta0.1O 3-δ (SCT10). The local crystal structure and oxygen stoichiometry of these materials were systematically characterized with in-situ neutron diffraction (ND). The oxygen stoichiometry was also measured by thermogravimetric analysis (TGA) and iodometric titration methods. To establish the correlation among structure, oxygen stoichiometry and oxygen reduction reaction (ORR) activity, high temperature electrochemical impedance spectroscopy, oxygen permeation and single cell testing were also performed. In chapter 2, SYC10 is described to have a more symmetrical structure and $V_o^{··}$ distribution, and higher $V_o^{··}$ concentration than SYC30. Molecular orbital energy analysis based on the local structure of the ORR-active Co1-polyhedra indicates SYC30 has a higher Fermi level relative to O-2p energy level in the active Co1-polyhedra, and thus a higher motional enthalpy for $V_o^{··}$ migration. However, the ORR activity of Y-doped SrCoO 3-δ (SCO) are found uncompetitive with other popular catalysts. In chapter 3 and 4, systematic structural studies are presented for Nb and Ta-doped SCO, namely SCN10 and SCT10, respectively. The methodology of unrevealing the structure-activity relationships in chapter 2 is also found applicable to SYC10, SCN10 and SCT10 as presented in chapter 5. The electrochemical tests indicate that SCT10 is the best catalyst due to its excellent thermal and electrochemical stability. In chapter 6, SCT10 is evaluated in a real solid oxide fuel cell in the form of nanoscaled SCT10 layer coating on the commercial (La 0.6 Sr 0.4 ) 0.95 Co 0.2 Fe 0.8 O 3-δ (LSCF). The bilayer structured cathode shows excellent properties of coarsening-resistant, Sr-segregation-free and high ORR-activity.

Yang, Tianrang↗

Comparative physiological and genomic characterization of a novel Nitrobacter vulgaris strain from a nitrate-contaminated subsurface

Nitrite-oxidizing bacteria (NOB) represent a crucial node in the global nitrogen cycle. By catalyzing the second step of nitrification—the oxidation of nitrite to nitrate to generate energy for growth—NOB activity controls the fate of nitrite (NO 2 - ) in aerobic environments. Despite thriving in diverse environments, including soils, freshwater, marine ecosystems, subsurface habitats, and water treatment systems, organisms capable of nitrite oxidation are confined to Nitrobacter, Nitrospira, Nitrospina, Nitrotoga, and a few other specific lineages. The genus Nitrobacter, recognized for its facultative heterotrophic metabolism, is often associated with high-nitrogen environments. Here, we report the physiological characterization of a novel strain, Nitrobacter vulgaris strain MLSD-S22, isolated from a nitrate- and heavy-metal-contaminated subsurface. Growth inhibition experiments revealed that strain MLSD-S22 and the N. vulgaris type strain Z exhibited similar sensitivities to nitrite and nitrate, with nitrite being the most inhibitory. Microrespirometry demonstrated that the two N. vulgaris strains and Nitrobacter winogradskyi Nb-255 possessed higher affinities for nitrite and oxygen than previously reported for Nitrobacter, suggesting potential to compete in low-substrate environments. Long-read DNA sequencing provided a complete genome for strain MLSD-S22, revealing two plasmids and an intact nitrous oxide (N 2 O) reduction operon—an unexpected feature for Nitrobacter. While N 2 O reduction activity was not observed under the tested conditions, this discovery raises questions about the contribution of Nitrobacter NOB to the N 2 O sink. These findings broaden the physiological and genomic diversity of Nitrobacter, offering new insights into their adaptation strategies and providing a framework for future evaluation of their potential roles in nitrogen loss.

Nitrobacter↗

Kinetically Controlled Synthesis of Rhodium Nanocrystals with Different Shapes and a Comparison Study of Their Thermal and Catalytic Properties

Here, we report the synthesis of Rh nanocrystals with different shapes by controlling the kinetics involved in the growth of preformed Rh cubic seeds. Specifically, Rh nanocrystals with cubic, cuboctahedral, and octahedral shapes can all be obtained from the same cubic seeds under suitable reduction kinetics for the precursor. The success of such a synthesis also relies on the use of a halide-free precursor to avoid oxidative etching, as well as the involvement of a sufficiently high temperature to remove Br – ions from the seeds while ensuring adequate surface diffusion. The availability of Rh nanocrystals with cubic and octahedral shapes allows for an evaluation of the facet dependences of their thermal and catalytic properties. The data from in situ electron microscopy studies indicate that the cubic and octahedral Rh nanocrystals can keep their original shapes up to 700 and 500 °C, respectively. When tested as catalysts for hydrazine decomposition, the octahedral nanocrystals exhibit almost 4-fold enhancement in terms of H 2 selectivity relative to the cubic counterpart. As for ethanol oxidation, the order is reversed, with the cubic nanocrystals being about three times more active than the octahedral sample.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Cascade Reaction of Ethanol to Butadiene over Ag-Promoted, Silica- or Zeolite-Supported Ta, Y, Pr, or La Oxide Catalysts

Ethanol converts to 1,3-butadiene in the presence of suitable multifunctional catalysts. In this work, Lewis acid cations Ta, Y, Pr, and La were dispersed on amorphous silica or beta zeolite, and after physically mixing with silica-supported Ag nanoparticles, were tested in the cascade reaction of ethanol to butadiene at 573 K. The Lewis acid catalysts were characterized by X-ray fluorescence, N 2 physisorption, scanning transmission electron microscopy (STEM), X-ray diffraction, diffuse reflectance (DR) UV-Vis and X-ray photoelectron spectroscopy. High-resolution STEM images confirmed the small oxide cluster size on the silica support. Results from DR UV-Vis spectroscopy showed zeolite-supported Ta and Pr catalysts had a smaller metal oxide cluster size, relative to their SiO 2 counterparts. X-ray photoelectron spectroscopy confirmed the oxidation state of the cations supported on the zeolite remained the same as that of their SiO 2 -supported analogues. The selectivity of the C 4 coupling products toward butadiene relative to butanol correlated with acid strength of the Lewis acid cations, as evaluated by the 2-propanol decomposition reaction to propene and acetone, with Ta being the most selective. In conclusion, the rate of C-C coupling over the zeolite-supported cations was enhanced by an order of magnitude compared to those cations supported on amorphous SiO 2 .

C-C bond formation↗

Minimizing Cr-Evaporation from Balance of Plant Components by Utilizing Cost-Effective Alumina-Forming Austenitic Steels

A solid oxide fuel cell (SOFC) is a clean and efficient energy conversion device. The development of intermediate-temperature SOFCs has made it preferable to use metallic interconnects (MICs) to greatly reduce the cost and significantly increase the efficiency compared to ceramic interconnect materials. However, gaseous chromium species will evaporate from the chromium-containing layer formed on the surface of commonly used MICs and balance of plant (BoP) components. Volatile chromium species have been shown to form solid deposits which poison the cathodes of SOFCs, causing drastic cell performance degradation and thereby limiting commercialization. In order to alleviate the Cr poisoning and achieve long-term high performance of SOFC stacks, various Al2O3-forming austenitic (AFA) stainless steels applied at different temperatures are evaluated in this project. Based on our Phase I results (500 h operation), it is shown that on the AFAs, an alumina-based protective layer forms under high temperature that is invulnerable to water vapor effects and suppresses the diffusion of chromium and manganese which can prevent the generation of spinels on the alloy surface. Therefore, 310S, OC4 and OC5 at 800 °C and 625, OC11 and OC11LZ at 900 °C are selected to be tested in the Phase II long-term operation. From the results, we find that besides the lower Cr evaporation rates and better oxidation resistance of AFAs than benchmark alloys after short-term (500 h) operation, AFAs also possess the sturdy and compact alumina layer after a long-term operation (5000 h). A protective oxide layer is of great importance for the long-term high-temperature operation of structural materials. The high-temperature oxidation behavior of AFAs and commercial 310S and 625 alloys in Air + 10% H 2 O at 800 °C and 900 °C is systematically investigated. Severe breakaway oxidation and minor spallation are observed for the 310S and 625 after the long-term operation, while the AFAs show high oxidation resistance. It is found that the formation of a continuous alumina layer could greatly prevent the volatilization of chromium vapors. In addition, the corresponding evolving models are discussed. Chromium evaporation from BoP components in high-temperature environment could severely deteriorate the electrochemical performance of SOFC. Several methods were applied to evaluate the Cr evaporation rates of BoP after 500 h exposure at 800 °C to 900 °C in air with 10% H 2 O. An optimal method was designed to exclude the effect of silicon (Si) deposits from quartz tube and sodium (Na) deposits from the sodium carbonate on the oxidation process and the chemical interaction between Cr gaseous species and alumina tube which could provide further quantitative correlation of the evaporated Cr species quantities and degradation rates of SOFC. Based on the great performance of AFAs after long-term operation, AFAs are assembled with Anode-supported cells (ASC) to investigate the the Cr deposition of anode-supported cell under a constant current density of 0.5 A cm -2 at 800 °C with AFA alloys compared with commercial alloys. In addition, the anodic and cathodic processes are deconvoluted by distribution of relaxation times (DRT) method which are comprehensively discussed. It is found out that the voltage exhibited a slight decrease of 5.09 % and 1.54 % in the presence of OC11 and OC11LZA alloy, respectively. However, a considerable decrease of 22.14 % and 12.06 % was determined in the presence of 310S and 625 alloy, respectively. AFAs possessing the low-cost, low Cr evaporation rates and the high oxidation resistance will make it of great potential to replace the existing BoP components.

36 MATERIALS SCIENCE↗

Minimizing Cr-Evaporation from Balance Of Plant Components By Utilizing Cost-Effective Alumina-Forming Austenitic Steels

A solid oxide fuel cell (SOFC) is a clean and efficient energy conversion device. The development of intermediate-temperature SOFCs has made it preferable to use metallic interconnects (MICs) to greatly reduce the cost and significantly increase the efficiency compared to ceramic interconnect materials. However, gaseous chromium species will evaporate from the chromium-containing layer formed on the surface of commonly used MICs and balance of plant (BoP) components. Volatile chromium species have been shown to form solid deposits which poison the cathodes of SOFCs, causing drastic cell performance degradation and thereby limiting commercialization. In order to alleviate the Cr poisoning and achieve long-term high performance of SOFC stacks, various Al 2 O 3 -forming austenitic (AFA) stainless steels applied at different temperatures are evaluated in this project. Based on our Phase I results (500 h operation), it is shown that on the AFAs, an alumina-based protective layer forms under high temperature that is invulnerable to water vapor effects and suppresses the diffusion of chromium and manganese which can prevent the generation of spinels on the alloy surface. Therefore, 310S, OC4 and OC5 at 800 °C and 625, OC11 and OC11LZ at 900 °C are selected to be tested in the Phase II long-term operation. From the results, we find that besides the lower Cr evaporation rates and better oxidation resistance of AFAs than benchmark alloys after short-term (500 h) operation, AFAs also possess the sturdy and compact alumina layer after a long-term operation (5000 h). A protective oxide layer is of great importance for the long-term high-temperature operation of structural materials. The high-temperature oxidation behavior of AFAs and commercial 310S and 625 alloys in Air + 10% H 2 O at 800 °C and 900 °C is systematically investigated. Severe breakaway oxidation and minor spallation are observed for the 310S and 625 after the long-term operation, while the AFAs show high oxidation resistance. It is found that the formation of a continuous alumina layer could greatly prevent the volatilization of chromium vapors. In addition, the corresponding evolving models are discussed. Chromium evaporation from BoP components in high-temperature environment could severely deteriorate the electrochemical performance of SOFC. Several methods were applied to evaluate the Cr evaporation rates of BoP after 500 h exposure at 800 °C to 900 °C in air with 10% H 2 O. An optimal method was designed to exclude the effect of silicon (Si) deposits from quartz tube and sodium (Na) deposits from the sodium carbonate on the oxidation process and the chemical interaction between Cr gaseous species and alumina tube which could provide further quantitative correlation of the evaporated Cr species quantities and degradation rates of SOFC. Based on the great performance of AFAs after long-term operation, AFAs are assembled with Anode-supported cells (ASC) to investigate the the Cr deposition of anode-supported cell under a constant current density of 0.5 A cm -2 at 800 °C with AFA alloys compared with commercial alloys. In addition, the anodic and cathodic processes are deconvoluted by distribution of relaxation times (DRT) method which are comprehensively discussed. It is found out that the voltage exhibited a slight decrease of 5.09 % and 1.54 % in the presence of OC11 and OC11LZA alloy, respectively. However, a considerable decrease of 22.14 % and 12.06 % was determined in the presence of 310S and 625 alloy, respectively. AFAs possessing the low-cost, low Cr evaporation rates and the high oxidation resistance will make it of great potential to replace the existing BoP components.

01 COAL, LIGNITE, AND PEAT↗

Mechanisms Engineering Test Loop (METL) Operations and Testing Report (FY2022)

This report documents the operations, testing, maintenance, and improvements that were performed at the Mechanisms Engineering Test Loop (METL) during FY2022. The METL facility had a very successful fourth year of operations and went through some new experiences such as taking the facility from its frozen state in October 2021 and thawing the facility and also recovering from an oxide plug in one of the cold trap lines. After the facility was fully thawed, the METL staff maintained the facility in a continuous molten state – either flowing sodium or a static flow condition. METL facility continued supporting the Gear Test Assembly (GTA) testing and hosted its first 28” test vessel experiment, called the Thermal Hydraulic Experimental Test Article (THETA) which was inserted into Test Vessel 4. Work to accommodate two additional experiments, a gripper test article (GrTA) and a flow sensor test article (F-STAr) continued as they are expected to make their debut in FY2023. In addition, the steam piping for the B308 scrubber unit was replaced with stainless steel piping and controls and new parts for the scrubber were purchased – such as a new pump, new storage tank, and new blower and motor. These components will ultimately replace the existing scrubber components when those 1970’s era require replacement.

42 ENGINEERING↗

On-Demand Designing of Cathode Internal Surface Architecture for Dramatic Enhancement of SOFC Performance and Durability

This project is aimed to design and modify the internal surfaces of porous composite cathode from currently commercially viable Solid Oxide Fuel Cells (SOFCs), using additive manufacturing process of Atomic Layer Deposition (ALD). The material systems being investigated are commercial composite electrodes complex three-dimensional topographies. In term of the chemistry of the ALD layer applied on the internal surface of the porous cathode, this project has employed commercially relevant electrolyte, electrocatalyst and noble metal materials set. Such materials are fully compatible with the commercial fuel cells, and this project has developed special nanostructure on the surface of the commercial composite cathodes. The formation of the designed nanoarchitecture on the surface of SOFC cathode has been achieved through precise control of ALD parameters and their effect on overall cell performance and resultant electrochemical reaction mechanism of cathodes has been investigated through full cell electrochemical performance testing and nanostructure characterization by transmission electron microscopy (TEM). Under the support of this award, following has been achieved: (1). For cathode materials in solid oxide fuel cells (SOFCs), such as perovskite mixed conductor La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3-x (LSCF), cation surface segregation and consequently losing conductivity and active sites for the oxygen reduction reaction (ORR) are problematic. To mitigate the cation segregation and enhance SOFC durability, further decorating the internal backbone surface using the desired electrocatalysts could be a promoting approach. Commonly, the cation segregation such as Sr is very volatile, so the effective surface decoration is ideally conformal. Nevertheless, the conformal surface coating would inevitably alter the ORR pathways that initially take place on the surface of the backbone. To reveal the impact of the conformal coating on both the catalytic activity and the conductivity of the cathode, the unary electrocatalyst of Pt or CoO x , was applied to the LSCF/SDC composite electrode of inherently functional SOFCs, respectively. Both ALD coating layers evolve strong interaction with the LSCF composite cathode. Upon operations, the Pt coating layer remains conformal on LSCF grain surfaces but turns into discrete particles on SDC grain surfaces. Meanwhile, CoO x conformal coating grows to be the discrete nanograins on both the LSCF and SDC grains. ALD coating of the cathode alone reduces the ohmic resistance up to 28 % for the entire cells. The increased conductivity induced by the ALD coating of Pt or CoO x is ascribed to different mechanisms. For the inherent functional SOFCs, the present study presents a novel and feasible approach to apply a conformal, dense coating layer on the surface of a mixed conductor, simultaneously increasing the conductivity and durability of the SOFC cathode. (2). High resistance of the oxygen electrode still significantly hinders the state-of-the-art Solid Oxide Fuel Cells (SOFCs). In particular, for an oxygen electrode consisting of mixed electronic and ionic conductors, such as perovskite lanthanum strontium cobalt ferrite (LSCF), it deteriorates due to its low chemical stability of the grain surface. Such degradation is often associated with the segregation of cations. To prevent the cation surface segregation and its resultant perovskite phase decomposition, we demonstrate a conformal ultra-thin (7-10 nm) surface heterogeneous coating layer consisting of subjacent discrete Pt nanoparticles capped with a superjacent fully dense conformal CoO x layer. The performance studies indicate the ALD coating reduces the cell series resistance by up to 40 %. The conformal CoO x layer consists of randomly orientated but single-layered nanograins, with high-density intergranular and surface grain boundaries serving as the electrochemical reaction sites and facilitating mass transport. The conformal coating layer appears to have successfully suppressed the Sr outward diffusion and confined the Sr enriched layer to a ~ 2 nm interface perovskite phase between the coating layer and the LSCF grain surface. Moreover, this ultra-thin Sr enriched perovskite layer presumably possesses high oxygen vacancy and high ionic conductivity and further imposes tensile strain to the LSCF grain surfaces. With the combination of a conformal CoO x nanoionics, Sr enriched layer, and its strained interface, the ALD coating induced surface layer is estimated to have a conductivity of ~ 1.27x10 4 S/cm, which is over two orders magnitude of that from LSCF at 750 ºC.

30 DIRECT ENERGY CONVERSION↗

Development of Chromium and Sulfur Getter for Solid Oxide Fuel Cell (SOFC) System

Under the “real world” SOFC operating conditions, gaseous Cr and S species coexist in air stream. The combined Cr and S effect on the electrochemical poisoning of candidate LSM and LSCF electrodes has been investigated. Electrochemical and structural analysis revealed that the combined Cr and S interactions with the LSCF electrode remains significantly different from those of the individual Cr and S interactions. S reacts with the surface SrO accompanied by morphological changes whereas the hexavalent gaseous Cr species mainly deposit at the LSCF/GDC interface as is the case with Cr-only poisoning. For LSM electrode, the combined interactions of Cr and S remains similar to the sum of individual Cr and S effects as SO 2 reacts with Sr-rich regions of the bulk LSM, while Cr deposits at the electrochemically active sites. The use of getter, consisting of alkaline earth and transition metal oxides, has been proposed as a cost-effective approach to mitigate electrode poisoning. SrMnO 3 (SMO) is suggested as a robust getter material for the co-capture of airborne gaseous S and Cr species entering high-temperature electrochemical systems. The honeycomb getter forms, covered with SMO nanoparticles, were fabricated using dip coating. The SMO getter successfully maintained the electrochemical activity of LSM under the presence of gaseous Cr and S species, validating the efficacy of the getter. Post-test characterization revealed that the absorption of S and Cr contaminants led to the elongation of granular SMO particles, forming SrO nanorods and SrCrO 4 whiskers leaving Mn oxides underneath where inward-migrating Cr reside, indicating the high mutual affinity of Sr and Mn. The growth of reaction products during the long term exposure favors continued absorption of incoming S and Cr contaminants. The Mn 2 O 9 dimers, existing on the surface, are considered to help absorb S and Cr impurities, along with the Sr-terminated surface. The SMO getter also displays robust stability in humid environments at high temperatures without phase transformation or hydrolysis, fulfilling the requirement for operation in high-temperature electrochemical systems.

30 DIRECT ENERGY CONVERSION↗

Analysis of iron-chromium-aluminum samples exposed to accident conditions followed by quench in the QUENCH-19 experiment

The QUENCH-19 experiment was a first-of-its-kind full-bundle test simulating accident conditions followed by water quench on accident-tolerant fuel (ATF) cladding. Here, a type of FeCrAl(Y) alloy, B136Y3, was developed at Oak Ridge National Laboratory and tested at the Karlsruhe Institute of Technology using Kanthal APM corner rods, a shroud, and Kanthal AF spacer grids. Testing conditions were similar to those in QUENCH-15—which tested ZIRLO cladding behavior—so that B136Y3 and ZIRLO cladding could be compared. QUENCH-19 consisted of an initial pre-oxidation heating followed by a transient. Then, a maximum power hold, which was not present in QUENCH-15, was executed to extend the heating period for the FeCrAl(Y) rods. Finally, a rapid water quench was executed that was similar to emergency core coolant system (ECCS) actuation. Compared with the ZIRLO rods in QUENCH-15, the bundle in QUENCH-19 released significantly less H 2 (9.2 g vs. 47.6 g) and achieved a much lower maximum temperature (1455°C vs. 1880°C). Furthermore, no breakaway oxidation was observed in QUENCH-19. Metallographic mounts revealed that despite the symmetry of the setup, at elevations near the maximum temperature, cladding and thermocouples were heavily damaged, substantial melting and oxidation occurred, and the cladding underwent chemical interaction with the thermocouple sheaths. Additionally, the ZrO 2 spacers detrimentally interacted with the cladding, leading to mixed oxide debris and the full destruction of some rods. Additional failure was found in certain cooler rods that may have risen due to the high thermal expansion coefficient of FeCrAl alloys. This paper presents an analysis of this work, which suggests that FeCrAl cladding can chemically survive anticipated loss-of-coolant accident events followed by rapid ECCS quench if the correct geometry and core design are present.

36 MATERIALS SCIENCE↗

Design of a Scavenging Pyrrole Additive for High Voltage Lithium-Ion Batteries

We report 1-(dimethylamino) pyrrole (PyDMA) as an electrolyte additive for high voltage lithium-ion batteries based on LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622)//Graphite with an upper cutoff voltage of 4.4 V. Density Functional Theory (DFT) modeling indicates that the unique structure of PyDMA could be effective in preventing the hydrolysis of LiPF 6 in a carbonate electrolyte, mitigating issues related to HF formation. The calculations also indicated that the additive would oxidize at lower potentials than typical electrolyte solvents, which could lead to protective films at the cathode surface. These expectations were tested using Nuclear Magnetic Resonance (NMR) and extensive electrochemical characterization. NMR studies confirmed the superb dehydrating capability of PyDMA, which successfully prevents HF formation even at high water content. Addition of 0.5 wt% PyDMA resulted in improved capacity retention in full-cells, and also in lower levels of transition metal dissolution from the cathode. Incremental capacity (dQ/dV) analysis indicates that benefits of PyDMA at low concentration (0.5–1 wt%) are associated with decreased rates of Li + -trapping reactions, and that higher concentrations of the additive can lead to isolation of cathode domains. Furthermore, our study indicates that PyDMA could be a promising electrolyte additive for high voltage lithium-ion batteries at a low concentration.

25 ENERGY STORAGE↗

Nitric oxide molecular tagging velocimetry of a free-flight model in a reflected shock tunnel

Nitric oxide molecular tagging velocimetry (NO MTV) is used to characterize the wake behind a free-flight spherical model in the test section of a free-piston reflected shock tunnel using a burst-mode laser operated at 100 kHz. A novel (to our knowledge) multi-delay timing scheme was implemented to measure velocity in a varying collisional environment in the wake of the free-flight model. Four simultaneous velocity profiles were measured in the wake of the model from -600 to 3600 m/s for flow enthalpies of 10.3 and 12.0 MJ/kg. Finally, the measured velocity distributions show good agreement when compared to computational fluid dynamics (CFD) modeling.

47 OTHER INSTRUMENTATION↗

Re-Additization of Commercial Biodiesel Blends During Long-Term Storage

Commercial biodiesel blends representative of the U.S. market were aged following procedure ASTM D4625, Standard Test Method for Middle Distillate Fuel Storage Stability at 43°C (110°F), with periodic monitoring of fuel properties indicative of oxidation. The oxidation stability—or oxidation reserve expressed as Rancimat induction period (IP)—gradually decreased from its initial value, as expected. At a predetermined IP threshold, an antioxidant was used to restore IP to the ASTM D7467 specification minimum of 6 six hours, referred to as re-additization. At lower IP values, the amount of antioxidant required increased significantly, and the effectiveness tended to be reduced. Once IP fell to essentially zero, the acid content increased to above the allowable limit. Insoluble material was detectable after the acid number increased out of specification. Storage life was increased with re-additization relative to the as-received fuels, as evidenced by longer time to produce acids. Experience in the field may vary based on storage conditions; however, these results indicate re-additization can significantly increase the storage life of biodiesel blends when used with regular monitoring of IP and acid number. An assessment of property changes during long-term storage showed the initial IP did not predict storage behavior, although fuels above the specification minimum remained stable for greater than 12 weeks of D4625 accelerated aging (1 one year simulated).

09 BIOMASS FUELS↗

Tank Side Cesium Removal IXC-150 Cask Detonation Report

A set of experiments were conducted at Los Alamos National Laboratory’s firing point 88 to determine the blast pressure and effects of a stoichiometric gas mixture of Hydrogen (H 2 ) and Nitrous Oxide (N 2 O) on the IXC-150 Storage Pad Vent Stack assemblies. The Lab was asked to design, build, and test the vent stack assemblies using a reaction gas volume of 340 in 3 that mimics the Tank Side Cesium Removal (TSCR) Ion Exchange Column (IXC) assembly. The experimental system with vent stack assembly was designed with input from the Washington River Protection Services (WRPS) to ensure an accurate test setup. The tests were conducted at LANL on the newly built filter/gas assembly at the end of April 2021 timeframe, using WRPS supplied vent stack assemblies and internal HEPA filters. The objective of these tests was to observe that the structural integrity of the vent stack assemblies was maintained and determine the resulting blast overpressures at a distance of 16 and 32 inches from the assembly. All work was performed under the LANL Quality Assurance Program (SD330), using a graded application of ASME NQA-1- 2008/NQA-1a-2009. To ensure that all client quality assurance (QA) expectations were addressed, evaluation of the end data needs was performed and the appropriate controls applied for this work.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Gypsum and clay-based additives to MSW for pre-combustion enhancement of syngas and solid residue improvement (Final Scientific/Technical Report)

This project was focused on the development of a cost-effective and practical approach for the recovery of metals and syngas from municipal solid waste (MSW) thermally processed in a gasification or combustion (i.e. waste-to-energy (WTE)) facility with the inclusion of other waste streams. The goal of additional waste inclusion was targeted to change the oxidation of critical and precious elements to enable them to be more efficiently recovered. The project had two main components: laboratory testing and techno-economic analysis (TEA). The additional waste included with MSW as gypsum and spent FCC (sFCC) catalyst as additives to improve material recovery and energy efficiency in MSW and WTE ash.

36 MATERIALS SCIENCE↗

Evidence for a High Temperature Whisker Growth Mechanism Active in Tungsten during In Situ Nanopillar Compression

A series of nanopillar compression tests were performed on tungsten as a function of temperature using in situ transmission electron microscopy with localized laser heating. Surface oxidation was observed to form on the pillars and grow in thickness with increasing temperature. Deformation between 850 °C and 1120 °C is facilitated by long-range diffusional transport from the tungsten pillar onto adjacent regions of the Y2O3-stabilized ZrO2 indenter. The constraint imposed by the surface oxidation is hypothesized to underly this mechanism for localized plasticity, which is generally the so-called whisker growth mechanism. The results are discussed in context of the tungsten fuzz growth mechanism in He plasma-facing environments. The two processes exhibit similar morphological features and the conditions under which fuzz evolves appear to satisfy the conditions necessary to induce whisker growth.

36 MATERIALS SCIENCE↗