Search NASA⌕ Search

SEARCH · Search NASA

Results for “surface analysis”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 703 records · Page 39
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

An organogel library for solution NMR analysis of nanoparticle suspensions in non-aqueous samples

Surface contrast solution NMR methods (scNMR) are emerging as powerful tools to investigate the adsorption of small molecule ligands to the surface of nanoparticles (NP), returning fundamental insight into the kinetics and thermodynamics of sorption, as well as structural information on the adsorbed species. A prerequisite for the acquisition of high quality solution NMR data is the preparation of homogeneous and stable samples that return consistent NMR spectra and allow extensive signal averaging. Unfortunately, this condition does not apply to NMR samples containing NPs that often show a tendency to sediment and accumulate at the bottom of the NMR tube over the course of the experiment. We have recently shown that preparing NMR samples in an agarose gel matrix inhibits sedimentation and allows the characterization of small molecule-NP interactions by scNMR. Unfortunately, as the agarose gel only forms in aqueous solution, this sample preparation method cannot be used to stabilize NP suspensions in a non-aqueous environment. In this work, we introduce a library of 48 organogels, based on low molecular-mass organic gelators (LMOGs), to prepare NMR samples of small molecule/NP systems in a wide range of organic solvents. In addition, we present a simple method that takes advantage of 1H transverse relaxation (1H-R2) measurements to screen the library and identify the best gelator to characterize the small molecule-NP interaction of interest in the solvent of choice. We expect the results of this study will enable the preparation of homogeneous and stable samples of NPs in non-aqueous environments, therefore dramatically increasing the applicability of scNMR to the characterization of heterogeneous interactions and to the investigation of the role played by solvent molecules in regulating the kinetics and thermodynamics of sorption.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Comparison of chromium poisoning between lanthanum strontium manganite and lanthanum strontium ferrite composite cathodes in solid oxide fuel cells

Degradation mechanisms of chromium poisoning have been extensively investigated for last two decades on various cathode materials for solid oxide fuel cells. While most researchers used half-cell experiments to investigate the effects of chromium impurities, this paper compares the degradation phenomena of LSM-YSZ and LSF-GDC cathodes in full cells under different operating conditions, namely polarized current density and humidity over the cathode. Under cathodic load, performance degradation of LSF-GDC cathode is significantly less than that of LSM-YSZ cathode. Most interestingly, under humidified air condition, LSF-based cell hardly experiences performance degradation while LSM-based cell shows a catastrophic degradation. Cr deposition in LSM-based cells occurs mainly near the electrolyte under both dry and humidified air conditions. In contrast, Cr deposition in LSF-based cell concentrates at the cathode surface under dry air condition, but concentrates both at cathode surface and near electrolyte under humidified air condition. Microstructure analysis reveals Mn-associated Cr deposits in LSM-based cathode, and Sr- and Fe-associated Cr deposits in LSF-based cathode. With the help of distribution of relaxation time analysis, the different electrochemical behaviors of LSM- and LSF-based cells are carefully interpreted. The effects of electrochemical deposition, Sr surface segregation, and humidity on LSM- and LSF-based cathodes are discussed.

25 ENERGY STORAGE↗
DOE OSTI2022

Removal of Bond Sodium from Full-Length Unirradiated Fermi-1 Blanket Elements and Assembly via Melt-Drain-Evaporate Process

Equipment was designed, fabricated, tested, and operated in an inert atmosphere radiological glovebox at Idaho National Laboratory to demonstrate the removal of bond sodium from full-length unirradiated Fermi-1 radial blanket elements and an entire radial blanket assembly using a Melt-Drain-Evaporate process. A series of three runs was performed with individual and multiple radial Fermi-1 blanket elements, and a fourth run was conducted with an entire Fermi-1 radial blanket assembly. After each run, the depleted uranium alloy slugs in every element slid out of its cladding, mechanically exhibiting the effectual absence of bond sodium. Quantitative and further qualitative analyses of the treated Fermi-1 material revealed the substantive, if not complete, absence of sodium metal in blanket element components. Indeed, entire columns of depleted uranium alloy slugs and associated cladding from select treated elements were separately contacted with water to react with residual sodium metal on the element surfaces, forming hydrogen gas. Samples of the resultant gas were analyzed to quantify the hydrogen concentration, which correlated to a residual sodium metal content for the treated element. Accordingly, no detectable sodium metal (<7 µg) was found on the surfaces of multiple depleted uranium alloy slugs after removal from its cladding. Detectable sodium metal, ranging from 14 to 30 µg, was found on the surfaces of one separated column of slugs and two separated full-length cladding segments. Each element originally contained ~25 g of bond sodium, resulting in quantitative sodium metal removal efficiencies of =99.9998%. The remaining separated uranium alloy slugs and cladding segments from the four runs were piece-wise immersed in alcohol while videorecording possible gas bubble formation as an additional qualitative analysis for residual sodium metal on treated surfaces, which identified the predominant absence of sodium reactivity on the balance of treated Fermi-1 blanket material. The results of this demonstration substantiate a path forward for treatment and disposal of 34 metric tons heavy metal of irradiated sodium-bonded Fermi-1 blanket material currently stored at Idaho National Laboratory.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Probing surface-adsorbate interactions through active particle dynamics

Adsorbate molecules present in a reaction mixture may bind to and block catalytic sites. Measurement of the surface coverage of these molecules via adsorption isotherms is critical for modeling and design of catalytic reactions on surfaces. However, it is challenging to measure isotherms in solution in a way that is directly relevant to catalytic activity under reaction conditions, particularly since adsorbates may bind with an enormous range of surface affinity parameters. Here we used the motion of self-propelled catalytic Janus particles, which employ the decomposition of hydrogen peroxide fuel as a propulsion mechanism, to determine the effective surface coverage of thioglycerol, furfural, and ethanol on a platinum surface as a function of concentration in aqueous solution by measuring the decrease in active motion due to the blocking of active sites. For strongly adsorbing thioglycerol, this effective coverage was compared and contrasted to the total adsorbed amount measured using inductively-coupled plasma analysis. Demonstrating the broad applicability of this approach, the surface affinity of the three adsorbates spanned more than four orders of magnitude. For each species, the adsorbate-mediated attenuation of active motion occurred over a wide concentration range and was well-described by a Langmuir isotherm. The strongly interacting thioglycerol had the highest affinity towards the surface (K a = 15.5 ± 4.3 mM –1 ) and fully deactivated the active particle motion at surface saturation. Furfural had an intermediate affinity (K a = 0.42 ± 0.07 mM –1 ) but did not fully block H 2 O 2 access to the surface at apparent saturation, consistent with a maximum fractional surface coverage of θ max = 0.67. Ethanol exhibited even lower affinity (K a = 0.0025 ± 2x10 -4 mM –1 ) and its coverage saturated at only θ max = 0.38. Analysis of isotherms at elevated temperatures enabled direct extraction of the enthalpies of adsorption. The degree of surface coverage at adsorbate saturation appeared to correlate with the relative energies of adsorption for the different adsorbate species and was consistent with adsorbate saturation of one of multiple active site populations towards H 2 O 2 decomposition. Furthermore, computational investigations into solvent effects on furfural adsorption showed good quantitative agreement with the experimental results. This work leverages unique properties of active particles to explore fundamental catalysis questions and demonstrates a novel paradigm for significant and experimentally accessible multidisciplinary research.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Impact of SO 2 on NiFe Nanoparticle Exsolution and Dissolution from LaFe 0.9 Ni 0.1 O 3 Perovskite Oxides

Ni-doped LaFeO 3 perovskite oxide is a promising cathode material for solid oxide electrolysis cells (SOECs) designed for CO 2 /H 2 O coelectrolysis. Here, the performance of LaFe 0.9 Ni 0.1 O 3 is being investigated under real-world conditions that include exposure to acid gases, such as SO 2 , relevant to SOEC operation. Experiments show that LaFe 0.9 Ni 0.1 O 3 exsolves NiFe nanoparticles, along with the formation of surface SO 4 2– and SO 3 2– after being exposed to 200 ppm of SO 2 . This suggests that the ionic diffusion of Ni 3+ and Fe 3+ between the bulk and the surface remains unaffected throughout the exsolution–dissolution–exsolution cycle. Thermochemical water splitting has been employed as a probe reaction to evaluate the catalytic properties of the exsolved NiFe nanoparticles. These nanoparticles demonstrated improved hydrogen production compared to bare perovskite oxide substrates. However, after exposure to SO 2 , the formation of Fe-rich NiFe nanoparticles led to poor thermocatalytic performance and rapid deactivation of the perovskite at elevated temperatures. Density functional theory (DFT) analysis was utilized to validate the experimental findings, indicating a significantly negative reaction energy for water splitting over exsolved Fe, as well as stronger binding of SO 2 to Fe than to Ni. Computational analysis further suggests that the presence of surface sulfate promotes the formation of Fe-rich NiFe nanoparticles, aligning with the experimental results. Overall, this study clarifies how SO 2 affects the structure of SOEC perovskite oxide candidate materials. Future engineering efforts should focus on enhancing nanoparticle exsolution and sulfur resistance, which is crucial for improving the hydrogen production capacity of La-based perovskite oxides for electro- and thermocatalytic water splitting in real environments containing acid gases.

Najimu, Musa [Univ. of Southern California, Los An↗
DOE OSTI2023

Development of an accelerator-based neutron source to prototype Mo-99 production, part I: A liquid LBE windowless target

In this article, Molybdenum-99 (Mo-99)’s decay product, technetium-99 (Tc-99 m), is one of the most critical isotopes for medical diagnostics. To provide U.S. domestic supply of Mo-99 without using high-enriched uranium (HEU), a subcritical uranium target assembly (UTA) is irradiated by an accelerator-based neutron source to create Mo-99 through fission. This study discusses the development of the accelerator-based neutron source. The high-energy electrons from the accelerator irradiate a liquid lead-bismuth eutectic (LBE) target to produce neutrons. Part I of this work focuses on numerical and experimental analysis towards the development of a liquid LBE windowless target. Unlike the existing windowless targets in literature, the current design creates a vertical free surface for a beam to irradiate. First, a hydrodynamic analysis of the LBE windowless target is performed. Simplified analytical calculations are assisted by 2D computational fluid dynamics (CFD) simulations to design the target, with the focus on eliminating recirculation zones and avoiding cavitation. With the optimized geometry, the experimental study is performed to investigate the flow hydrodynamics using liquid LBE. The experiments (1) compare pressure drop in the system to correlation predictions; (2) visualize the free surface liquid LBE flow from the beam view; (3) validate the LBE flow profile using temperature sensitive paint from the side view; and (4) validate the liquid LBE film thickness using gamma densitometer measurements. Second, the power handling capability of the designed windowless target is investigated. The divider plate in the current design is susceptible to overheating due to the thin LBE film in front. As LBE erosion and corrosion is likely to occur at an LBE velocity of 2.0 m/s and temperature above 500 °C, a power limit of 10 kW of beam power was established to prevent this corrosion from occurring, which is calculated by a Nusselt number correlation. The divider plate surface temperature at 10 kW agrees well with the 3D CFD simulation results. Part I demonstrates the fundamental physics in liquid LBE windowless target design and associated testing. A companion paper, Part II will demonstrate how to couple this windowless target into the Mo-99 production system, including an accelerator system operating under an ultra-high vacuum and the UTA cooled by water at room temperature.

43 PARTICLE ACCELERATORS↗
DOE OSTI2024

Dynamic Scaling Analysis of Accelerated Irradiation Testing on Additive Manufacturing Materials by Positron Annihilation

The timely applications of Additive Manufacturing (AM) materials in nuclear environments require accelerated irradiation tests, mainly ion irradiation to enable rapid prototyping. Low dose ion irradiation would cause sub-nanostructure changes by generation of lattice defects, vacancies, vacancy clusters and voids and void swelling caused by cellular dislocations. Positron Annihilation Lifetime (PAL), a novel technology, sensitive towards sub-nanostructure morphology with high accuracy (about 10-7 vacancy per atom), supported by Transition Electron Microscope (TEM) would be applied to identify the type and total size of the defects. The subsequent PAL measurements and TEM surface studies would be followed by PAL analysis that includes sophisticated trapping model. The PAS results would become an input to dynamic scaling analysis (that predicts radiation effects from low dose studies for high dose effects), which incorporate mean-field theory model. The final effect is an in-depth understanding of the microstructure evolution of AM materials under ion irradiation which can be extrapolated to the studies of neutron irradiation, since ion-irradiation takes less time and do not cause the irradiation hazard. The working hypothesis is that PAL technology, that have excellent sensitivity to low-defect concentration would help to identify ion-induced material damage on the atomic and nano-scale level, which then could be extrapolated to understand the neutron damage better.

accelerated irradiation testing↗
DOE OSTI2026

Calcium Gradient-Doped LiNi 0.5 Mn 1.5 O 4 Cathode for Long Cycle Life Lithium-Ion Batteries

High-voltage spinel LiNi 0.5 Mn 1.5 O 4 (LNMO) has attracted considerable attention as a cathode material for next-generation lithium-ion batteries due to its high operating voltage and intrinsically fast lithium-ion diffusion kinetics. However, the practical implementation of LNMO remains limited by its rapid capacity decay, primarily associated with bulk structural instability and parasitic interfacial reactions. To address these issues, we innovatively introduced calcium (Ca) as a dopant to enhance both the oxygen framework and surface stabilities of the LNMO crystal through gradient doping. Observations from the electronic microscopies, X-ray diffraction, and the elemental analysis confirmed that Ca is preferentially enriched at the particle surface, and a disordered crystal phase is preserved in the bulk in the gradient-doped LNMO cathodes. As cathodes in LIBs, the Ca gradient-doped (Ca gr) LNMO materials delivered formation capacities of ∼126−130 mAh/g and exhibited Coulombic efficiencies of 88−95%, which are consistently higher than those of the uniform-doped samples at the same doping level and undoped sample. Especially, the Ca gr 0.05 LNMO cathode demonstrated significantly improved rate capability with ∼113 mAh/g preserved at 10 C, while ∼92 mAh/g and ∼110 mAh/g for undoped and Ca uniform 0.05 LNMO, respectively, and excellent cycling stability, retaining ∼124.1 mAh/g (∼96.3% capacity retention) after 500 cycles. The analysis of cyclic voltammetry, differential capacity, and electrochemical impedance revealed that the excellent electrochemical performance is attributed to the structural and morphological advantages of gradient-doped LNMO cathodes with a disordered bulk structure for fast Li + diffusion and a Ca-enriched surface for minimizing the Mn dissolution.

25 ENERGY STORAGE↗
DOE OSTI2024

Development of the tangent linear and adjoint models of the global online chemical transport model MPAS-CO 2 v7.3

We describe the development of the tangent linear (TL) and adjoint models of the Model for Prediction Across Scales (MPAS)-CO 2 transport model, which is a global online chemical transport model developed upon the non-hydrostatic Model for Prediction Across Scales – Atmosphere (MPAS-A). The primary goal is to make the model system a valuable research tool for investigating atmospheric carbon transport and inverse modeling. First, we develop the TL code, encompassing all CO 2 transport processes within the MPAS-CO 2 forward model. Then, we construct the adjoint model using a combined strategy involving re-calculation and storage of the essential meteorological variables needed for CO 2 transport. This strategy allows the adjoint model to undertake a long-period integration with moderate memory demands. To ensure accuracy, the TL and adjoint models undergo vigorous verifications through a series of standard tests. The adjoint model, through backward-in-time integration, calculates the sensitivity of atmospheric CO 2 observations to surface CO 2 fluxes and the initial atmospheric CO 2 mixing ratio. To demonstrate the utility of the newly developed adjoint model, we conduct simulations for two types of atmospheric CO 2 observations, namely the tower-based in situ CO 2 mixing ratio and satellite-derived column-averaged CO 2 mixing ratio (X CO 2 ). A comparison between the sensitivity to surface flux calculated by the MPAS-CO 2 adjoint model with its counterpart from CarbonTracker–Lagrange (CT-L) reveals a spatial agreement but notable magnitude differences. These differences, particularly evident for X CO 2 , might be attributed to the two model systems' differences in the simulation configuration, spatial resolution, and treatment of vertical mixing processes. Moreover, this comparison highlights the substantial loss of information in the atmospheric CO 2 observations due to CT-L's spatial domain limitation. Furthermore, the adjoint sensitivity analysis demonstrates that the sensitivities to both surface flux and initial CO 2 conditions spread out throughout the entire Northern Hemisphere within a month. MPAS-CO 2 forward, TL, and adjoint models stand out for their calculation efficiency and variable-resolution capability, making them competitive in computational cost. In conclusion, the successful development of the MPAS-CO 2 TL and adjoint models, and their integration into the MPAS-CO 2 system, establish the possibility of using MPAS's unique features in atmospheric CO 2 transport sensitivity studies and in inverse modeling with advanced methods such as variational data assimilation.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Spotlight: efficient automated global optimization in rietveld analysis of diffraction data

Performing reliable Rietveld analysis on tens or hundreds of powder diffraction datasets from parametric or time-resolved experiments often poses a bottleneck in extracting meaningful results from the data. While automated analysis of data has recently been demonstrated, high temperature annealing studies, during which phase transformations occur and lattice parameters may change due to repartitioning of elements, are prime examples where automation by a simple phase identification from a database of room temperature structures or automation by sequential refinements is likely to fail. To enable reliable, efficient, automated Rietveld analysis, we present a Python package named Spotlight , building on established Rietveld packages such as MAUD, GSAS , or GSAS-II , which extends the refinement of best fit parameters to a global optimization using an ensemble of optimizers leveraging hierarchical parallel execution on high-performance computing clusters. Spotlight further enables the efficient design of refinement plans through the iterative automated machine-learning of a surrogate for the refinement on which the global optimizations are performed until results from the surrogate converge to the response surface data. We demonstrate Spotlight with the analysis of uranium molybdenum and Ti–6Al–4V datasets, as well as in two open-source tutorials analyzing aluminium oxide and lead sulphate.

36 MATERIALS SCIENCE↗
DOE OSTI2021

ExoMars Mars Organic Molecule Analyzer (MOMA) Laser Desorption/Ionization Mass Spectrometry (LDI-MS) Analysis of Phototrophic Communities from a Silica-Depositing Hot Spring in Yellowstone National Park, USA

The Mars Organic Molecule Analyzer (MOMA) is a key scientific instrument on the ExoMars Rover mission. MOMA is designed to detect and characterize organic compounds, over a wide range of volatility and molecular weight, in samples obtained from up to two meters below the martian surface. Thorough analog sample studies are required to best prepare to interpret MOMA data collected on Mars. We present here the MOMA characterization of Mars analog samples collected from an alkaline silica depositing hot spring in Yellowstone National Park, WY, USA. These samples contain microbial streamer communities composed primarily of oxygenic and anoxygenic phototrophs. Additionally, in a study focused on detection of key classes of nonvolatile organics, samples of microbial streamers and their total lipid extract (TLE) have been measured on a MOMA Engineering Test Unit (ETU) instrument using its laser desorption/ionization mass spectrometry (LDI-MS) mode. MOMA LDI-MS detected a variety of lipids and pigments in the TLE sample. Species such as chlorophyll a were also detected from the streamer sample with the help of mass isolation. The results add to the LDI-MS sample characterization database, as well as demonstrate the benefit of using mass isolation on the MOMA instrument to reveal the presence of complex organics, and potential biomarkers, preserved in a natural sample, providing guidance to the in situ analysis of surface samples during Mars operations.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Measurement of isosteric heat of gas adsorption and Brunauer–Emmett–Teller (BET) surface area using a quartz crystal microbalance

The study of gas adsorption on a solid surface evaluates the affinity between sorbate gas and sorbent substrate and factors that contribute to this. This report presents a test platform for adsorption experiments of various gases on various solid surfaces. Controlled environmental conditions enable investigations in materials surface science and increase the consistency among adsorption data. The system utilizes a quartz crystal microbalance to perform gravimetric analysis of deposition and adsorption, enabling investigation of the interaction of gaseous molecules with solid surfaces. In this study, a quartz crystal microbalance as gas adsorption detector was integrated with an environmental chamber to create a versatile tool for gas adsorption experiments on thin films. Experimental operation of this apparatus was demonstrated via acquisition of the adsorption isotherms of cyclohexane vapor on a gold surface at 55 and 70 °C. The result indicated International Union of Pure and Applied Chemistry Type II adsorption. Consequentially, application of the Brunauer–Emmett–Teller model to the isotherm data subject to predefined criteria for linear region selection yielded a surface area of the sorbent of 0.53 cm2 at 55 °C. From the monolayer region of the isotherms, the isosteric heat of adsorption of the cyclohexane vapor on gold was calculated to be 37 kJ mol-1.

47 OTHER INSTRUMENTATION↗
DOE OSTI2025

Monitored Natural Attenuation (MNA) Assessment for the Chemicals, Metals, and Pesticides (CMP) Pits Operable Unit (OU) and the Pen Branch Wetland

In October 2024, Savannah River National Laboratory (SRNL) was tasked to conduct an independent review of groundwater data and assess the monitored natural attenuation (MNA) performance related to the Chemicals, Metals, and Pesticides (CMP) Pits Operable Unit (OU) located in the central portion of the Savannah River Site (SRS). The SRNL assessment of MNA entailed an independent analysis of groundwater concentration data, groundwater elevation data, available surface water concentration data, soil concentration data, and relevant historical geological characterization logs for the CMP Pits OU. Historical data tables and records were obtained from both the Savannah River Nuclear Solutions - Area Completion Projects (SRNS&#x2;ACP) team and South Carolina State University (SCSU) and condensed into new data sets by the SRNL project team for more targeted analysis of MNA performance characteristics. All data pertaining to groundwater concentration, surface water concentration, and groundwater elevation were restricted to collection dates after any known active remediation for the CMP OU.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

The Radius of PSR J0740+6620 from NICER with NICER Background Estimates

We report a revised analysis for the radius, mass, and hot surface regions of the massive millisecond pulsar PSR J0740+6620, studied previously with joint fits to NICER and XMM-Newton data by Riley et al. (2021) and Miller et al. (2021). We perform a similar Bayesian estimation for the pulse-profile model parameters, except that instead of fitting simultaneously the XMM-Newton data, we use the best available NICER background estimates to constrain the number of photons detected from the source. This approach eliminates any potential issues in the cross-calibration between these two instruments, providing thus an independent check of the robustness of the analysis. The obtained neutron star parameter constraints are compatible with the already published results, with a slight dependence on how conservative the imposed background limits are. A tighter lower limit causes the inferred radius to increase, and a tighter upper limit causes it to decrease. We also extend the study of the inferred emission geometry to examine the degree of deviation from antipodality of the hot regions. We show that there is a significant offset to an antipodal spot configuration, mainly due to the non-half-cycle azimuthal separation of the two emitting spots. The offset angle from the antipode is inferred to be above 25° with 84% probability. This seems to exclude a centered-dipolar magnetic field in PSR J0740+6620.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2020

Accuracy in Resolving the First Hydration Layer on a Transition-Metal Oxide Surface: Experiment (AP-XPS) and Theory

Understanding the equilibrium conditions at the metal oxide/aqueous interface is a key component toward visualizing the structure of water in confined environments and differentiating the catalytic activity of transition-metal oxides. While ambient pressure X-ray photoelectron spectroscopy (AP-XPS) has been the primary technique to investigate the formation of a hydration layer on many surfaces, results over the extended relative humidity (RH) range accessible experimentally have not been compared quantitatively to theoretical predictions. With the use of first-principles theoretical methods and accumulated knowledge of AP-XPS spectral analysis, we do so here for a model surface, TiO 2 -terminated undoped SrTiO 3 (100) (STO). The measured distribution of OH and H 2 O coverages from vacuum up to the first hydration layer is in good agreement with a static density functional theory (DFT) configuration involving partial dissociation of H 2 O per Ti-atom mediated by H-bonding. Furthermore, ab initio molecular dynamics (AIMD) simulations at 300 K for select coverages (1/4, 1/2, and 1 ML) test the role of fluctuations and entropy in the competition between adsorption and dissociation with coverage. This comparison between theory and experiment for OH and H 2 O coverages on STO provides a foundation for a more quantitative assessment of the first hydration layer and associated competition between adsorption, dissociation, and H-bonding on transition-metal oxide surfaces.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Mechanical Loads on Spent Nuclear Fuel in the General 30 cm Package Drop Scenario

The U.S. Department of Energy Office of Nuclear Energy (DOE-NE) Spent Fuel and Waste Science & Technology (SFWST) research program is guided by the high-level goal of closing prioritized knowledge gaps related to spent nuclear fuel (SNF) storage and transportation, which are summarized by Saltzstein et al. (2020). One of the high-priority knowledge gaps is the identification and quantification of mechanical loads that are expected to affect SNF during normal conditions of transportation and storage to inform the range of physical SNF test programs. This report uses modeling and analysis methods to estimate the mechanical loads on spent nuclear fuel (SNF) in the general 30 cm package drop scenario. The drop scenario assumes impact limiters are in place in the transportation configuration and the impact surface is perfectly rigid. The goal of this analysis is to consider the universe of potential mechanical loading conditions that can happen to SNF and present the results in a manner that is useful for materials testing, decision making, and regulatory rule making purposes. This study uses validated finite element models and methods to perform a broad parametric study of key variables that can affect the mechanical loads on SNF during a hypothetical package free drop scenario. Physical drop test data from a cask and fuel assembly drop test campaign is the basis for model validation. Additionally, the results of the parametric study are used to inform a damage model, which uses multiple nonlinear regression to estimate the relationships between input variables and output response. The parametric finite element analyses consider thousands of input variable combinations, while the damage model estimates millions of combinations. The breadth of this study provides confidence that the potential range of mechanical loads that SNF might experience during the general 30 cm package drop scenario are characterized well enough to consider this knowledge gap closed. While this report documents the overall peak values calculated in this study, the 95 th percentile values, the histograms, and the observed trends are equally important. This study covered a large range of SNF temperatures, room temperature to 300°C, and burnups, 10 GWd/MTU to 62 GWd/MTU. Each temperature and burnup combination has a different cladding yield strain, so it is more meaningful to summarize the calculated cladding strain response as its factor of safety, which is defined relative to the yield strain. The factor of safety is calculated as the yield strain divided by the peak cladding strain. A factor of safety greater than unity indicates that the cladding remains below yield, whereas a value less than unity is indicative of plastic deformation. In all cases of this study a safety factor over 1.0 was calculated, although in the most limiting case at 300°C the safety factor was only 1.01, which suggests that yielding could occur when additional loads like rod internal pressure are included. When the temperature is restricted to 200°C the limiting safety factor increases to 1.28, which has significant margin to accommodate internal pressure and potential local cladding defects that could cause a local stress concentration. An important trend in the calculated fuel rod mechanical loads is that the 2 nd highest loaded fuel rod in an assembly tends to be significantly lower than the highest loaded rod. The implication is that even if one rod in an assembly experiences a failure the loads would have to be significantly higher to cause two or more rods to fail.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

Microchannel-based Membrane-less Extraction of Li from Unconventional Lithium Sources & the Separation of REE

This final report provides an overview of the Project's entire duration, covering July 1, 2021 to December 31, 2023. It primarily focuses on the achievements, technological developments, and unique challenges the team faced while working on separating and extracting Lithium from produced waters. The project's primary aim was to create an integrated, high-throughput, membrane-less, and modular microfluidic platform that could extract Lithium from unconventional sources. We have successfully met all goals and milestones envisioned in the SOPO document. The most critical primary milestones, including the Go-No-Go milestone (refer to the Gantt chart in the Appendices), were successfully accomplished. We demonstrated phase separation (>90%) and extraction (>85%) performance in the MPSE using synthetic, and representative produced water composition feed at 50 ml/min total flow through MPSE 36. We have also performed a parametric study of the MPSE operations, beyond the scope of SOPO, exploring operating conditions of current and broader interest. The extended investigation of operational parameters is concurrent with our efforts to seek further development of the MPSE technology beyond the scope of the Project. Along these lines of development, we have made efforts to be responsive to DOE calls for technological developments of other types of resources (beyond PW) for the recovery of Critical Materials and higher TRL development (beyond TRL 4). During the work on this Project, we developed and implemented three innovative technical approaches that emerged from our efforts to successfully meet the Project milestones. The innovative & original technical approaches developed and implemented in this Project are now the contributions to process engineering that could be clearly credited to the Project. First, Convergent Design Approach is a comprehensive feedforward & feedback loop of four design phases: i) design for functionality, ii) design for manufacturing, iii) design for sustainability, and iv) design for market. Next was Process Intensification. A major aim of this Project was to create an innovative phase separation & extraction microscale-based technology for Li separation – thus the words microchannel-based in the Project title. A microscale-based technology is intrinsically in the center of the Process Intensification domain as defined by its unique principles. Therefore, Process Intensification was implicitly envisioned in the Project’s SOPO. Lastly, Time Scale Analysis is a novel tool for discovering the needs and directions of Process Intensification implementations in any process technology. This Project is fully credited for developing and implementing the three novel technical approaches mentioned above. These are general contributions to process engineering that emerged from this Project. Beyond the original SOPO scope, the OSU-U.Pitt research group utilized a Convergent Design methodology, integrating first-principles mathematical modeling with experimental validation on the Minimum Development Vehicle. By creating these Digital Twins, the team rapidly assessed manufacturing iterations to support TEA analysis. This framework further enabled the development of advanced Surface Modification Techniques, where hydrophobic and oleophobic coating strategies were optimized via Digital Twin tools and validated through rigorous 100-hour longevity testing. TEA Analysis: The closing efforts of this Project were focused on the TEA analysis. TEA analysis had two primary functions: i) enabling critical assessments of design variations withing 10 the Concurrent Design Approach, thus enabling evolution of the MPSE design to reach faster- better-cheaper alternatives; and ii) to create a bridge between the accomplishments of this Project and future projects of higher TRL, beyond TRL 6 level. It is important to note that the TEA model created in the Project stirred the technological solutions for the recovery of critical materials toward a vision of a very profitable modular plant that has unique zero-waste water discharge signature. More importantly, thanks to our experimental performance data and conservative assumptions, the TEA model predicts minimal technological and investment risks. Low cost of a modular unit of a nominal capacity of [1000 tons of Li 2 CO 3 /year] positions the MPSE based technology within the reach of community investors, thus offering a paradigm shift in the development of critical technologies. The project successfully navigated two primary challenges: solvent selection and manufacturing adaptation. Restricted by the SOPO to existing literature for lithium recovery, the team identified a critical need for a "material excellence program" to develop next-generation solvents, eventually concluding with a preliminary investigation into promising Ionic Liquids (ILs). Simultaneously, COVID-19 supply chain disruptions forced a pivot from traditional manufacturing to advanced additive methods at ATAMI-OSU. By transitioning from stainless steel to 3D-printed polymer substrates, the team achieved a transformative three-order-of- magnitude reduction in manufacturing costs and compressed prototyping timelines from several months to just two days. The MPSE technology offers significant energy, environmental, and economic advantages by overcoming the traditional bottlenecks of phase-separation hardware and contactor size. Unlike conventional mixer-settlers or membrane-based systems, MPSE operates without moving parts or fouling-prone membranes, achieving robust performance even with challenging, viscous, or particulate-heavy feeds. Key performance metrics include an energy intensity reduction of 5–50x (3–40 kJ/m 3 ) compared to incumbent technologies and a dramatic reduction of processing time to under 60 seconds, which drastically reduces the physical plant footprint. These technical efficiencies translate into superior economic outcomes; for a 100 t/year Li 2 CO 3 facility, implementing MPSE is projected to nearly halve contactor CAPEX (from $\$$6.08M to $\$$3.01M) and significantly increase the project's Net Present Value (NPV), derisking new investment and enabling distributed critical-mineral processing configurations. The commercialization of MPSE technology is being spearheaded by Vigsur Dynamics Inc., which has adopted a structured, parallel approach to technical and business development since its formation in January 2026. Following extensive customer discovery and engagement with the Oregon State University accelerator, Vigsur Dynamics is working to establish a business model that transitions from pilot demonstrations to modular hardware sales, ultimately aiming for a "build-own-operate" service strategy. Current technical milestones—including 100 hours of continuous operation, superior energy efficiency, and successful 6-unit modular scale-up— provide a foundation for this transition. Backed by ongoing IP licensing and a growing network of industrial and venture advisors, the company is actively de-risking the platform to replace conventional mixer-settler systems in the critical minerals market.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗