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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.

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At least 127 records · Page 7
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Exploring the First High-Entropy Thin Film Libraries: Composition Spread-Controlled Crystalline Structure

Thin films of two types of high-entropy oxides (HEOs) have been deposited on 76.2 mm Si wafers using combinatorial sputter deposition. In one type of the oxides, (MgZnMnCoNi)O x , all the metals have a stable divalent oxidation state and similar cationic radii. In the second type of oxides, (CrFeMnCoNi)O x , the metals are more diverse in the atomic radius and valence state, and have good solubility in their sub-binary and ternary oxide systems. Therefore, the resulting HEO thin films were characterized using several high-throughput analytical techniques. The microstructure, composition, and electrical conductivity obtained on defined grid maps were obtained for the first time across large compositional ranges. The crystalline structure of the films was observed as a function of the metallic elements in the composition spreads, that is, the Mn and Zn in (MgZnMnCoNi)O x and Mn and Ni in (CrFeMnCoNi)O x . The (MgZnMnCoNi)O x sample was observed to form two-phase structures, except single spinel structure was found in (MgZnMnCoNi)O x over a range of Mn > 12 at. % and Zn < 44 at. %, while (CrFeMnCoNi)O x was always observed to form two-phase structures. Composition-controlled crystalline structure is not only experimentally demonstrated but also supported by density function theory calculation.

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

Nanotomography for Quantitative 3D Particle Reconstruction

Particulates are ubiquitous across fuel cycle operations and carry critical information about particle formation, processing, and potential proliferation-related activities. Traditional analytical techniques, including micro-Raman spectroscopy and standard electron microscopy, are often limited in spatial resolution or dimensionality, particularly when used to examine metallic or submicron-scale features. Understanding particle morphology, phase distribution, and internal porosity is essential for constraining formation conditions, thermodynamic environments, and material transport behavior. In this report, we demonstrate the application of plasma focused ion beam nanotomography to reconstruct micron-scale particulates at nanoscale resolution. Using high-resolution backscattered electron imaging and Avizo software, we obtained 3D reconstructions that enabled quantitative analysis of particle morphology, phase composition, and internal voids. Representative examples include a Ta particle with a large central void and a composite particle with embedded tetrahedral crystalline structures. These reconstructions reveal structural and compositional details that are inaccessible through conventional 2D imaging. The results demonstrate that nanotomography provides both qualitative and quantitative insights into particle formation and behavior. Using nanotomography, porosity and phase distributions can be quantified to inform models of particle density, transport, and solidification conditions. Beyond technical insights, the workflow developed here establishes a transferable capability for analyzing heterogeneous particles and has potential applications in bulk materials studies via x-ray computed tomography or other volumetric imaging modalities. Ongoing efforts are focused on optimizing the workflow to process multiple particles simultaneously, increasing throughput and statistical robustness. Overall, this work illustrates the power of nanotomography as a tool for connecting particulate morphology to formation mechanisms, composition, and transport, thereby strengthening analytical capabilities for nuclear forensics, fuel cycle analysis, and related scientific investigations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

Investigating the Impacts of Aqueous-Phase Processing on Organic Aerosol Chemical Climatology Using ARM and ASR Observations

This project improved understanding of how atmospheric aerosol particles form and evolve, with a focus on the role of water-driven (aqueous-phase) chemical reactions in the atmosphere. These processes occur in clouds, fog, and humid air and can significantly change the composition and properties of airborne particles, known as aerosols, which influence air quality and climate. By combining field measurements, laboratory experiments, and advanced analytical techniques, the project identified key chemical signatures that allow scientists to distinguish particles formed through aqueous processes from those formed in the gas phase. Observations from multiple environments, including wildfire smoke, urban regions, and cloud-influenced areas, show that aqueous chemistry is an important pathway for particle formation and aging. The project also developed new measurement approaches using uncrewed aerial systems (UAS) to capture how aerosol composition varies with altitude, providing critical insights into how particles interact with clouds. In addition, new data analysis frameworks were created to better interpret long-term aerosol measurements and improve characterization of particle sources and transformations. These results have been integrated into a global database of aerosol measurements and used to support atmospheric modeling efforts. Overall, the project provides important tools and knowledge to improve predictions of how aerosols affect climate and air quality, particularly through their interactions with radiation and clouds.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Understanding Trace Iron and Chromium Incorporation During Gibbsite Crystallization and Effects on Mineral Dissolution

Incorporation of pollutants, e.g., heavy metals, or critical elements, e.g., lithium, as impurities in mineral phases can significantly affect their mobility or sequestration in the environment. Even when present at low concentrations, impurities can alter the solubility and reactivity of the host mineral. Here, in this study, we investigate the incorporation of trace amounts of iron (Fe 3+ ) and chromium (Cr 3+ ) during the crystal growth of the aluminum (Al 3+ ) hydroxide, gibbsite, a major component of bauxite ores, an important soil mineral, and a dominant mineral phase in stored radioactive wastes. Using a comprehensive suite of analytical techniques, we show that both Cr 3+ and Fe 3+ can be incorporated into the gibbsite lattice during coprecipitation by replacing Al 3+ in octahedral sites. These small amounts are consistent with limited to no structural isomorphism shared between Al 3+ and Cr 3+ /Fe 3+ hydroxide precipitates, nor room temperature miscibility of their isostructural M 2 O 3 oxide forms, in contrast with oxyhydroxide forms where Al 3+ and Fe 3+ share similar structural topologies. Despite the limited uptake of Cr 3+ /Fe 3+ , we show that these impurities have significant implications for gibbsite dissolution behavior. The limited uptake of Cr 3+ /Fe 3+ (e.g. 0.43% Cr 3+ and 0.4% Fe 3+ ), we show that these impurities have significant implications for gibbsite dissolution behavior and subsequent reactivity in complex environments.

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

Pilot-scale hydrotreating of catalytic fast pyrolysis biocrudes: process performance and product analysis

Catalytic fast pyrolysis (CFP) is a technology option for producing advanced biofuels from hydrocarbon-rich biocrude intermediates. The relatively high oxygen content of biocrudes compared to petroleum intermediates increases hydrogen consumption and the lower thermal stability accelerates catalyst deactivation and reactor fouling hindering the adaptation of hydrotreating technology for biocrude upgrading into biofuels. In this study, four chemically different biocrude feeds were upgraded in a pilot scale hydroprocessing unit at similar process conditions using a commercial hydrodeoxygenation (HDO) catalyst. The biocrude feeds and hydrotreated products were characterized using standard ASTM procedures and advanced analytical techniques (GCxGC-FID and GCxGC-MS). HDO catalyst activity was monitored by changes in physical properties and chemical composition of the upgraded products as a function of time on stream. Aliphatic acids, ketones, aldehydes, and furan derivatives were completely converted during the hydrotreating tests while the concentration of aromatics, aliphatic hydrocarbons and phenolics increased during the hydrotreating tests. The oxygen content, nitrogen content, specific gravity, viscosity and the heavy end of the boiling point range (determined by simulated distillation) of the upgraded products increased with increasing time on stream during hydrotreating. The deactivation rate was the lowest for the biocrude feed that contained the most aliphatic and aromatic hydrocarbons and was the highest for the biocrude feed that had the most anhydrosugars. Overall, the HDO deactivation rate correlates with the total amount of oxygen in the feed (17 wt% to 29 wt%, on a wet basis).

09 BIOMASS FUELS↗
DOE OSTI2020

Influence of chain length in protic ionic liquids on physicochemical and structural features of lignins from sugarcane bagasse

We report the mechanisms behind lignin dissolution with protic ionic liquids (PILs) and their influence over lignin properties remain not fully explored. In this work, physicochemical and structural features of lignins extracted from sugarcane bagasse after pretreatment with a series of PILs (length of the cation chain combined with different anions) were assessed using analytical techniques. It was found that the lignin extracted with shorter chain length cations PILs showed the highest β-O-4 content. Opposite, the increase of the PILs cation chain length resulted in enhanced depolymerization. All lignins presented high polydispersity (>3.7), while the weight average molecular ranged from 1921 to 13,539 g/mol. The recovered [Eti][Mal] lignin presented the higher β-O-4 content and was possibly the most preserved lignin obtained. Opposite, lignin isolated from [Hex][Ac] and [Hex][For] treatments had less β-O-4 linkages attributed to the depolymerization of lignin via rupture of ether linkages generating intermediates that further repolymerized and/or depolymerized. These results suggest that the ionicity of the PIL is a crucial factor for lignin dissolution. Furthermore, these results illustrate that the proposed pretreatment using different PILs is useful to obtain high-quality lignins with distinct features and opens a new perspective for materials to match various applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Impact of Boron-Containing Lubricant Additive on Three-Way Catalyst Reactivity and Physicochemical Properties

Boron-containing compounds are one of the lubricant additive options due to their suitable properties for additives and have been used as commercial lubricant additives. In the present study, the impact of a boron-containing lubricant oil additive, AR9100 (BR), on Pd/Rh-based three-way catalyst (TWC) performance is investigated, and the results are compared with the baseline no-additive (NA) case and the industry standard zinc dialkyl-dithiophosphate (ZDDP) results. Accelerated engine aging is performed using a genset to expose the catalysts to lubricant additives at high temperatures. All aged TWC samples are investigated for reactivity in a bench-flow reactor and characterized using a variety of analytical techniques. Compared with the no-additive case, the temperatures of 90% conversion (T 90 ) of NO, CO, C 3 H 6 , and C 3 H 8 for the ZDDP-aged TWC sample increased by 34, 30, 37, and 48 °C. However, the T 90 of all gas species for the BR-aged TWC sample are similar to the NA-aged TWC sample. Additionally, a significant decrease in water–gas shift reactivity and oxygen storage capacity is observed in the ZDDP-aged sample, but not in the BR-aged sample. Inductively coupled plasma-optical emission spectrometry (ICP-OES) analysis and electron probe microanalysis (EPMA) maps of accelerated engine aging samples show the presence of phosphorus and boron in ZDDP- and BR-aged TWC samples, respectively. However, no boron-related peaks are observed in the X-ray diffraction (XRD) pattern of the BR-aged TWC sample, which may exist in the form of an amorphous phase.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

High resolution mobility spectrometry in a co-axial platform

Ion mobility spectrometry is an analytical technique that separate ions in the gas phase based on their interaction with a neutral buffer gas. Ion mobility spectrometry performs separations quickly (typically less than a second) and the ion mobilities are very reproducible across different laboratories. This project aimed at evaluating the performance of a new ion mobility device. The new device relies on conducting ion mobility separation in a curved geometry. The project explored the operation landscape of the device using ion trajectory simulations then fabricated and experimentally demonstrated the device's performance. Ion trajectory simulations on a set of tetraalkylammonium and phosphazene ions indicate that ions traveling a curved path length undergo mobility separation that is similar to a straight path. The ion mobility resolution of the curved device was found to be similar to that of a straight path of a similar length. The experimental validation of the new device confirmed the device's ability to separate ions according to their mobilities. Sets of mixtures (tetraalkylammonium ions, phosphazene ions, and peptide ions) were evaluated for separation and transmission.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

A review on recent machine learning applications for imaging mass spectrometry studies

Imaging mass spectrometry (IMS) is a powerful analytical technique widely used in biology, chemistry, and materials science fields that continue to expand. IMS provides a qualitative compositional analysis and spatial mapping with high chemical specificity. The spatial mapping information can be 2D or 3D depending on the analysis technique employed. Due to the combination of complex mass spectra coupled with spatial information, large high-dimensional datasets (hyperspectral) are often produced. Therefore, the use of automated computational methods for an exploratory analysis is highly beneficial. The fast-paced development of artificial intelligence (AI) and machine learning (ML) tools has received significant attention in recent years. These tools, in principle, can enable the unification of data collection and analysis into a single pipeline to make sampling and analysis decisions on the go. There are various ML approaches that have been applied to IMS data over the last decade. Here, in this review, we discuss recent examples of the common unsupervised (principal component analysis, non-negative matrix factorization, k-means clustering, uniform manifold approximation and projection), supervised (random forest, logistic regression, XGboost, support vector machine), and other methods applied to various IMS datasets in the past five years. The information from this review will be useful for specialists from both IMS and ML fields since it summarizes current and representative studies of computational ML-based exploratory methods for IMS.

47 OTHER INSTRUMENTATION↗
DOE OSTI2025

An In Situ , Automated High-Explosives Aging Method Utilizing Two-Dimensional Gas Chromatography–Mass Spectrometry

Understanding chemical changes that occur in high explosives as they age is of great importance to the safe employment and storage of these compounds. Traditional methods of aging high explosives even under accelerated aging conditions are time intensive with durations on the order of months to years. The nature of traditional aging analyses reduces each sample to a snapshot data point often separated widely in time, requiring many assumptions as to how the degradation products develop. Further complicating matters, several analytical techniques are typically employed for each sample analysis in order to ascertain an entire picture of the decomposition pathways. To address these shortcomings with existing methods, a new method of accelerated aging of high explosives utilizing comprehensive two-dimensional gas chromatography coupled to high-resolution mass spectrometry (GC × GC-HRMS) was developed using 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (CL-20) as a model compound for method development. This in situ automated method reduces the time scale of aging to a matter of hours using the inlet of the GC × GC as the aging vessel. GC × GC in combination with HRMS allowed for the collection of both evolved gases and other decomposition products produced during the entire aging process in real time with HRMS providing far greater certainty in identification of explosives aging products. Additionally, this method allowed for a higher throughput of samples with greatly simplified sample preparation. Chemometric analysis of the GC × GC-HRMS data set via the alteration analysis (ALA) enabled discovery of statistically significant chemical changes providing insight into the variation of decomposition pathways with varying aging temperatures.

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

Influence of the Anionic Zinc-Adeninate Metal–Organic Framework Structure on the Luminescent Detection of Rare Earth Ions in Aqueous Streams

Rare earth elements (REEs) are critical to numerous technologies; however, a combination of increasing demand, environmental concerns, and monopolistic marketplace conditions has spurred interest in boosting the domestic REE production from sources such as coal utilization byproducts. The economic viability of this approach requires rapid, inexpensive, and sensitive analytical techniques capable of characterizing the REE content during resource exploration and downstream REE processing (e.g., analyzing REE separation, concentration, and purification production steps). Luminescence-based sensors are attractive because many REEs may be sensitized to produce element-specific emission. Hence, a single material may simultaneously detect and distinguish multiple REEs. Metal–organic frameworks (MOFs) can sensitize multiple REEs, but their viability has been hindered by sensitivity and selectivity challenges. Understanding how the MOF structure impacts the REE sensing efficacy is critical to the rational design of new sensors. Here, we evaluate the sensing performance of seven different anionic zinc-adeninate MOFs with different organic linkers and/or structures for the visible-emitting REEs Tb, Dy, Sm, and Eu. The choice of a linker determines which REEs are sensitized and significantly influences their sensitivity and selectivity against competing species (here, Fe(II) and HCl). For a given linker, structural changes to the MOF can further fine-tune the performance. The MOFs produce some of the lowest detection limits (sub-10 ppb for Tb) reported for the aqueous sensitization-based REE detection. Importantly, the most selective MOFs demonstrated the ability to sensitize the REE signal at sub-ppm levels in a REE-spiked acid mine drainage matrix, highlighting their potential for use in real-world sensing applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Elucidating the local structure of Li 1+ x Al x Ti 2– x (PO 4 ) 3 and Li 3 Al x Ti 2– x (PO 4 ) 3 ( x = 0, 0.3) via total scattering

Li 1+x Al x Ti 2–x (PO 4 ) 3 (LATP) and Li 3 Al x Ti 2–x (PO 4 ) 3 (x = 0, 0.3) are promising candidates in all-solid-state batteries due to their high room temperature conductivity of 10 –3 S cm –1 and air- and moisture-stability. They also exhibit unusual thermal expansion properties, with Li 1+x Al x Ti 2–x (PO 4 ) 3 showing near-zero thermal expansion along the a axis while Li 3 Al x Ti 2–x (PO 4 ) 3 exhibits polynomial positive thermal expansion along the a axis and polynomial negative thermal expansion along the c axis. A crucial component to understanding these properties is understanding the local structure. Total scattering is a powerful analytical technique as it provides information on the long-range, average structure as well as the local structure. Here, we report the first X-ray and neutron total scattering experiments performed on Li 1+x Al x Ti 2–x (PO 4 ) 3 and Li 3 Al x Ti 2–x (PO 4 ) 3 (x = 0, 0.3). We show that the PO 4 and TiO 6 polyhedra experience very little expansion of the P/Ti–O bonds up to 800 °C, nor is there much expansion when the Li content increases significantly. The minor thermal expansion of the nearest-neighbor bonds of the polyhedra is revealed to be the reason behind the unusual thermal expansion properties, causing the near-zero thermal expansion along a in Li 1+x Al x Ti 2–x (PO 4 ) 3 and moving as whole units in Li 3 Al x Ti 2–x (PO 4 ) 3 . The structural robustness of the framework is also the reason for the increased conductivity as Li content increases, as the framework remains undistorted as Li content increases, permitting Li-ion mobility as the number of charge carriers increases. Finally, this suggests that phosphate-based framework materials beyond LATP would also be a good material space to explore for new Li-ion (and other ion-) conducting materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Chiral Spectroscopy of Nanostructures

Chirality is ubiquitous in the universe and in living creatures over detectable length scales from the subatomic to the galactic, as exemplified in the two extremes by subatomic particles (neutrinos) and spiral galaxies. Between them are living creatures that display multiple levels of chirality emerging from hierarchically assembled asymmetric building blocks. Not too far from the bottom of this pyramid are the foundational building blocks with chiral atomic centers on sp 3 carbon atoms exemplified by L-amino acids and D-sugars that are self-assembled into higher-order structures with increasing dimensions forming highly complex, amazingly functional, and energy-efficient living systems. The organization and materials employed in their construction inspired scientists to replicate complex living systems via the self-assembly of chiral components. Multiple studies pointed to unexpected and unique electromagnetic properties of chiral structures with nanoscale and microscale dimensions, including giant circular dichroism and collective circularly polarized scattering that their constituent units did not possess. To address the wide variety of chiral geometries observed in continuous materials, singular particles, and their complex systems, multiple analytic techniques are needed. Simultaneously, their spectroscopic properties create a pathway to multiple applications. For example, mirror-asymmetric vibrations at chiral centers formed by sp 3 carbon atoms lead to optical activity for the infrared (IR) wavelength regions. At the same time, understanding the optical activity in, for example, the IR region enables biomedical applications because multiple modalities of biomedical imaging and vibrational optical activity (VOA) of biomolecules are known for IR range. In turn, VOA can be realized in both absorption and emission modalities due to large magnetic transition moments, as vibrational circular dichroism (VCD) or Raman optical activity (ROA) spectroscopy. In addition to the VOA, in the range of longer wavelengths, lattice vibrational mode or phononic behavior occurs in chiral crystals and nanoassemblies, which can be readily detected by terahertz circular dichroism (TCD) spectroscopy. Meanwhile, chiral self-assembly can induce circularly polarized light emission (CPLE) regardless of the existence of chirality in coassembled fluorophores. The CPLE from self-assembled chiral materials is particularly interesting because the CPLE can originate from both circularly polarized luminescence and circularly polarized scattering (CPS). Furthermore, because self-assembled nanostructures often exhibit stronger optical activity than their building blocks owing to dimension and resonance effects, the optical activity of single assembled nanostructures can be investigated by using microscopic technology combined with chiral optics. Here, we describe the state of the art for spectroscopic methods for the comprehensive analysis of chiral nanomaterials at various photon wavelengths, addressed with special attention given to new tools emerging both for materials with self-organized hierarchical chirality and single-particle spectroscopy.

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

In-situ monitoring of atomically dispersed Pt sites supported on OMS-2 during CO 2 activation

Atomically dispersed catalysts have drawn great interest lately, as they showcase a high density of active sites, selectivity, and high turnover frequencies in oxidation chemistry due to labile oxygen activation. In contrast, the applications of these catalysts have lagged in reduction reactions due to the ambiguity caused by the sintering and restructuring of active sites. To bridge this gap, the evolution of Pt 4+ isomorphically substituted into an octahedral molecular sieve structure (OMS-2) under reductive conditions was correlatively characterized using multiple in-situ analytical techniques such as ambient pressure X-ray photoelectron spectroscopy, environmental transmission electron microscopy, and solid-state nuclear magnetic resonance. The surface dynamics of the Pt single atoms were revealed during the Reverse Water Gas Shift (RWGS) reaction, where the active sites were identified as two-coordinated platinum single atoms. Under reaction, we show nonbinding atoms adjacent to the single atoms restructured the motif of the single atoms to Pt 2+ via ion mobility of potassium, increasing the activation energy by 25.6 kJ/mol. Here, this work also highlights the potential for increased stability of the single atom sites via isomorphic substitution of the metal oxide support, since the Pt-OMS-2 catalyst retained activity for about 33 h before deactivation, after which nanoparticles were observed in TEM images. This work offers a new perspective in single atom synthesis using the metal oxide as the host for the single atom site, instead of adatoms on the surface

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Ion Mobility Spectrometry-Mass Spectrometry for High-Throughput Analysis

Ion mobility spectrometry is a widely used analytical technique providing gas phase separation of molecules. It has received increasing attention in the recent years with the advancement in technology development and the availability of commercial instruments. In this chapter, we introduced the ion mobility fundamental theory and provided examples of IMS applications, especially for isomer separation, collision cross section database generation, high throughput analysis workflows, software tools for IMS data analysis, and ongoing high resolution SLIM IMS development. While IMS is not yet routinely utilized in drug discovery and pharmaceutical industry, there has been increased interest in high throughput library screening and antibody characterization. With all the ongoing development in IMS technology and informatics, we foresee more and more exciting applications of high throughput IMS analysis in different fields including omics studies, drug discovery and clinical applications in the near future.

Ross, Dylan H.↗
DOE OSTI2020

Investigating the Effects of Chemical Gradients on Performance and Reliability within Perovskite Solar Cells with TOF-SIMS

Time-of-flight secondary-ion mass spectrometry (TOF-SIMS), a powerful analytical technique sensitive to all components of perovskite solar cell (PSC) materials, can differentiate between the various organic species within a PSC absorber or a complete device stack. The ability to probe chemical gradients through the depth of a device (both organic and inorganic), with down to 100 nm lateral resolution, can lead to unique insights into the relationships between chemistry in the absorber bulk, at grain boundaries, and at interfaces as well as how they relate to changes in performance and/or stability. In this essay, the technique is described; then, from the literature, several examples of how TOF-SIMS have been used to provide unique insight into PSC absorbers and devices are covered. Finally, the common artifacts that can be introduced if the data are improperly collected, as well as methods to mitigate these artifacts are discussed.

14 SOLAR ENERGY↗
DOE OSTI2020

Mapping of Heterogeneous Catalyst Degradation in Polymer Electrolyte Fuel Cells

Pt catalysts in polymer electrolyte fuel cells degrade heterogeneously as the catalyst particles are exposed to local variations throughout the catalyst layer during operation. State-of-the-art analytical techniques for studying degradation of Pt catalysts do not possess fine spatial resolution to elucidate such non-uniform degradation behavior at a large electrode level. A new methodology is developed to spatially resolve and quantify the heterogeneous Pt catalyst degradation over a large area (several cm ) of aged MEAs based on synchrotron X-ray microdiffraction. PEFC single cells are aged using voltage cycling as an accelerated stress test and the degradation heterogeneity at a micrometer length scale is visualized by mapping Pt catalyst particle size after voltage cycling. It is demonstrated in detail that the Pt catalyst particle size growth is non-uniform and follows the flow field geometry. The Pt particle size growth is greater in the area under the flow field land, while it is minimal in the area under the flow field channel. Additional non-uniformity is observed with the Pt particle size increasing more rapidly at the air outlet area than the Pt particle size at the inlet area.

36 MATERIALS SCIENCE↗
DOE OSTI2020

In situ liquid SIMS analysis of uranium oxide

Trace analysis of nuclear materials in solid particles collected in the environment or particles in liquid slurry generated in nuclear material manufacturing processes can pinpoint elemental, organic, and isotopic signatures of nuclear fuel cycle activities and processes. Such information can support nuclear safeguards programs by increasing our ability to detect undeclared nuclear materials, routine activities for safeguarding at declared facilities, and illicit activities. However, trace radioactive material analysis in liquids and slurries is challenging using bulk approaches. For example, one drawback of sensitive analysis such as inductively coupled plasma mass spectrometry (ICP-MS) is that sample is consumed or destroyed as a result of the technical approach. We developed a vacuum compatible microfluidic interface to enable surface analysis of liquids and liquid-solid interactions using time-of-flight secondary ion mass spectrometry (ToF-SIMS). In this work, we illustrate initial results of liquid standards containing uranium using in situ liquid SIMS. Specifically a series of diluted uranium standards used for ICPMS analysis were studied and the limit of detection was estimated. Since the liquid SIMS analysis is almost nondestructive, the same sample can be analyzed by other more destructive approaches afterwards or saved for future references. Consequently, multimodal analysis is possible. Our results demonstrate that in situ liquid SIMS can be used as a new approach to analyze radioactive materials in liquid and slurry forms of relevance to the IAEA safeguards missions.

In situ liquid ToF-SIMS, uranium, limit of detecti↗