Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “Oxidation Testing”

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 271 records · Page 15
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Photo-oxidation of semicrystalline polymers: Effect of stress triaxiality on ductility

The effect of stress triaxiality on the strain-to-fracture of as-received and photo-oxidized polyamide-6 (PA-6) was investigated using mechanical testing, synchrotron X-ray tomography, and finite element analyses. Mechanical tests were conducted on cylindrical and round notched specimens, where different notch radii were used to vary the stress triaxiality. The specimens were aged by exposure to ultra-violet (UV) radiation at 60∘, causing photo-oxidation. As-received and so-aged specimens were loaded to failure (complete loss of load carrying capacity). For both unaged and aged specimens, a higher triaxiality led to a lower strain-to-fracture. To elucidate the micromechanical damage that mediates fracture in both conditions, specimens with an intermediate notch sharpness were loaded to the peak load, unloaded, and scanned ex situ using synchrotron X-ray tomography. Damage in the unaged bar was found to occur by cavitation and was concentrated at the center of the specimen, where the triaxiality is highest. In the UV-aged bar, a network of inter-connected chemical cracks were found on the notch surface, where the triaxiality is lowest. Finite element analyses were deployed to approximate the local triaxiality at damaged regions in the unaged and UV-aged specimens using a constitutive relation for semicrystalline polymers. From these analyses, the relationship between local triaxiality and strain-to-fracture was quantified for both unaged and photo-oxidized PA-6. Both unaged and photo-oxidized PA-6 showed similar decreases in ductility with triaxiality, hinting at common ductile fracture processes.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Microscale mechanical property variations of Al-substituted LLZO: insights from compression testing and molecular dynamics simulations

Ceramic solid electrolytes based on LLZO (Li 7 La 3 Zr 2 O 12 ) are promising candidates for all-solid-state batteries due to their high ionic conductivity and good apparent stability vs. lithium metal, however they are prone to mechanical failure. Lithium metal intrusions, alongside cell stack pressure, transition polycrystalline solid electrolyte grains into a compressed state that promotes crack propagation and fracture. Here this work examines the mechanical response of Al-substituted LLZO to compressive forces by measuring ultimate strength under pillar compression with a flat punch tip. Failure modes characterized by in situ scanning electron microscopy show diverse splitting patterns arising from internal porosity, grain boundaries, and slip planes. Large correlated variations in compressive strength (0.93–2.63 GPa) and Young's modulus (72.1–150.97 GPa) are observed across microscale regions of the solid electrolyte. Molecular dynamics simulations of LLZO with different porosities describe the variation of compressive strength and Young's modulus, and enable a microscale porosity model to be fit accounting for Young's modulus reduction across the solid electrolyte. Overall, the results indicate the importance of microscale mechanical testing of ceramic solid electrolytes to identify preferential sites for mechanical degradation and Li intrusion, and ensure the robust design of all-solid-state lithium metal batteries.

25 ENERGY STORAGE↗
DOE OSTI2020

Elevated temperature mechanical properties of Inconel 617 surface oxide using nanoindentation

Inconel 617 is a principal candidate material for helium gas cooled very-high-temperature reactors with outlet temperatures of 700–950 °C. Recent findings showed that this alloy develops unique surface oxide layers especially at high temperature (HT) helium environment with distinctive wear, friction and contact properties. This study investigates the elevated temperature mechanical properties of Inconel 617 top surface layers aged in HT helium environment. Nanoindentation technique is used to obtain load-displacement graphs of the alloy top surface oxide in temperatures ranging from 25 °C up to 600 °C. In addition, using finite element analysis along with an iterative regression technique, a semi-numerical method is developed to further measure and quantify the material parameters and, in particular, time-independent and creep characteristics of the oxide. Although Young's modulus of the oxide is found to be relatively close to the bulk for the tested temperatures, the yield strength and hardness, in comparison to the bulk material, increase significantly as the material is oxidized after aging. The oxide exhibits significant softening as the temperature increases to 600 °C. Unlike the bulk material, diffusion through the grains is found to be the dominant creep mechanism for the oxide. Considerable difference between the mechanical properties of the oxide and the bulk material shows the need for accurate measurements of near surface mechanical properties, if reliable predictive contact and tribological models are sought at elevated temperatures.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Strength and rupture geometry of un-irradiated C26M FeCrAl under LOCA burst testing conditions

Ferritic iron-chromium-aluminum (FeCrAl) alloys are an accident tolerant fuel candidate to replace the incumbent Zr-based claddings. Nuclear grade FeCrAl alloys are marked by superior high temperature mechanical behavior and exceptional steam oxidation resistance, both of which increase safety margins during accident scenarios. In the present study, the loss of coolant accident (LOCA) burst behaviors of three un-irradiated commercially fabricated cladding materials in a simulated LOCA environment were compared: (1) T35Y2, a 1 st generation nuclear grade FeCrAl, (2) C26M, a 2 nd generation nuclear grade FeCrAl, and (3) Zircaloy-2. Both FeCrAl alloys showed improved mechanical strength and steam oxidation resistance compared to Zircaloy-2. C26M claddings burst at significantly higher temperatures for all tested engineering hoop stresses, had limited ballooning, and demonstrated preferential fuel retention behavior in terms of burst opening area and length. High temperature tensile data for C26M is also presented. For both un-irradiated FeCrAl alloys, it was found that a distinct “threshold” burst stress signified the transition between small and large openings. Finally, higher threshold hoop stresses were associated with higher uniaxial strength for the FeCrAl alloys, indicating that tensile data, rather than creep data, could be useful for predicting rupture size and assessing fuel dispersal concerns.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Parametric Study of Used Nuclear Oxide Fuel Constituent Dissolution in Molten LiCl-KCl-UCl 3

Prior work identified dissolution of used nuclear oxide fuel constituents from a uranium oxide matrix into molten LiCl-KCl-UCl 3 at 500°C, prompting a subsequent series of three progressive studies (including an initial scoping study, an electrolytic dissolution study, and a chemical-seeded dissolution study) to further investigate associated parameters and mechanisms. Thermodynamic calculations were performed to identify possible reaction mechanisms and their propensities in used oxide fuel constituent dissolution. Used nuclear oxide fuels with varying preconditions from fast and thermal test reactors were separately immersed in the subject salt system to assess fuel constituent migration from the bulk fuel matrix to the salt phase in an initial scoping study. Dissolution of expected fuel constituents, including alkali, alkaline earth, lanthanide, and transuranium oxides, into the chloride salt phase varied widely, ranging from 12% to 99% in the initial study. Uranium isotope blending between the salt phase and bulk fuel matrix was also observed, which was attributed to reducing conditions in the fuel matrix. Electrolytic and chemical-seeded dissolution studies were subsequently performed to effect reducing conditions in the fuel. Other parameters, including temperature (at 500°C, 650°C, 725°C, and 800°C) and uranium trichloride concentrations (at 6, 9, and 19 wt% uranium), were investigated in the latter two studies, resulting in fuel constituent dissolution above 90%. Extents of dissolution were based on initial and final fuel constituent concentrations in the oxide fuels following operations in the salt and subsequent removal of the salt via distillation. Finally, in this series of progressive studies, oxide fuel preconditioning and in situ reducing conditions, along with elevated temperature and uranium trichloride concentrations, were the primary parameters promoting used nuclear oxide fuel constituent dissolution in accordance with identified reaction mechanisms.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

SQMS science advances impact on Rigetti commercial processors

The collaboration between the Superconducting Quantum Materials and Systems Center (SQMS) and Rigetti Computing produced several advancements in our understanding of the role of materials characteristics in quantum processor performance. This partnership leverages SQMS's extensive characterization infrastructure and cutting-edge research in materials, and Rigetti's expertise in quantum hardware and robust nanofabrication to improve precision and performance of Rigetti's test QPUs. Qubit frequency is determined in large part by the properties of Josephson junctions (JJs) made of amorphous oxide tunnel barriers; the Alternating-Bias Assisted Annealing (ABAA) process allows us to tune JJs to their desired frequency [1]. Work by SQMS researchers in characterizing high-precision JJs post-processed (using ABAA) have yielded crucial information on the nature of the structure and chemical bonding uniformity of the ABAA processed amorphous oxides. Performance has also been improved through a comprehensive series of experiments that tested encapsulation and surface treatment. Encapsulation of the niobium metal layer with tantalum resulted in an T1 improvement of 80%, experimentally confirming the role of Nb surface losses in qubit performance [2]. Pre-treatment of the underlying silicon surface prior to JJ fabrication by replacing a buffered oxide etch (BOE) with hydrofluoric acid (HF) followed by aqueous ammonium fluoride (NH4F) has shown a statistically significant improvement of T1 by 22%, and reduction in the number of strongly-coupled TLS [3]. These examples, as well as many other published and ongoing investigations, demonstrate the mutual benefits that come from Rigetti's involvement in the SQMS collaboration. [1] - Pappas, D.P., et al. (2024). https://doi.org/10.1038/s43246-024-00596-z [2] - Bal, M., et al. (2024). https://doi.org/10.1038/s41534-024-00840-x [3] Kopas, C. J. et al. Preprint at https://doi.org/10.48550/arXiv.2408.02863 (2024).

Lachman, Ella↗
DOE OSTI2026

A comparative study of multimodal data fusion strategies for planetary spectroscopy

Integrating heterogeneous data sources can improve scientific inference when different modalities capture complementary information, but doing so is challenging in high-dimensional, small-sample settings. In spectroscopy for planetary exploration, Laser-Induced Breakdown Spectroscopy (LIBS), Raman Spectroscopy (Raman), Visible Infrared Spectroscopy (VISIR), and Mid-Infrared Spectroscopy (MIR) each examine different aspects of composition and mineralogy, raising fundamental questions about when and how data fusion improves predictive performance. Using a Mars-relevant set of geologic standards with measurements from all four modalities, we present a rigorous systematic evaluation of four data fusion strategies: low-level (data) fusion, mid-level (feature) fusion, high-level (decision) fusion, and residual-boosting (sequential) fusion. We assess performance in predicting oxide composition via nested cross-validation and corrected significance testing to evaluate whether data fusion improves upon single-modality baselines. We show that data fusion does not uniformly improve accuracy, and that observed gains are modest, oxide-dependent, and sensitive to modality and model structure. To move beyond aggregate accuracy metrics, we use model coefficients, permutation importance, and residual gain analysis to examine how the fusion models weight individual modalities and to identify patterns of apparent complementarity or redundancy. Though focused on spectroscopy for planetary exploration, our framework for data fusion evaluation and interpretation extends to other scientific domains with heterogeneous and scarce data and provides a principled approach evaluating data fusion strategies, interpreting modality contributions, and understanding tradeoffs among data fusion strategies.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2025

The Development of Catalysts for Upgrading of Pyrolysis Vapor for Refinery Feedstocks and Intermediates (CRADA Final Report)

Catalytic fast pyrolysis (CFP) is a versatile technology platform to convert biomass into fungible hydrocarbon transportation fuels and chemical co-products. Key technical barriers to reaching this goal include increasing the product yields and achieving the desired fuel properties for gasoline, diesel, and jet range fuels or blendstocks that would be suitable for introduction into existing refinery unit operations. Overcoming these barriers will require durable catalysts that are effective at upgrading and stabilizing biomass pyrolysis vapors. Towards these goals, this CRADA leveraged NREL experience as a leader in biomass pyrolysis research and Johnson Matthey's (JM) experience as a leader in the production of advanced catalytic materials. The scope spanned CFP catalyst development, characterization, multi-scale reaction testing, and computational modeling. CRADA benefits to DOE, Participant, and U.S. Taxpayer: Assists laboratory in achieving programmatic scope, Uses the laboratory’s core competencies. The purpose of this CRADA was to develop and deploy catalysts for biomass CFP to help achieve cost-competitive biofuels and bio-based products. This was accomplished through a close collaboration between biomass conversion researchers at NREL and catalyst development researchers at JM. Summary of Research Results: Focus Area 1. Foundational research on catalytic conversion and deactivation: Key interactions between pyrolysis vapors and heterogeneous catalysts were probed through catalyst characterization, model compound reaction testing, and atomistic-scale computational modeling. Catalyst development focused on multifunctional materials, which include zeolites, oxides, carbides, and nitrides. Computational modeling identified reaction mechanisms and elucidated surface chemistry to test hypotheses regarding mechanisms of deoxygenation, coupling, cracking, dehydration, coke formation, hydrogen transfer, and aromatic ring reactions. This information was used to design multifunctional catalysts to increase product yields, control product selectivity, and reduce deactivation during CFP and downstream processing steps. The results served to increase fundamental understanding of key catalyst attributes and durability features for the upgrading of biomass pyrolysis vapors. Model compound experiments confirmed the importance of metal-acid bifunctionality for the deoxygenation of lignin-derived phenolic species under hydrodeoxygenation conditions. This insight led to the development of catalysts such as Pt/TiO2 and Mo2C, which were confirmed as high-performing materials during subsequent bench-scale experiments using biomass-derived pyrolysis vapors. This focus area also led to the identification of important catalyst deactivation mechanisms associated with the deposition of inorganic contaminants such as potassium. The molecular-level insight from model compound experiments and computational modeling, shown in Figure 1, informed the development of regeneration procedures that have been shown to be effective for restoration of > 90% of initial catalyst activity. This understanding has subsequently been translated to other catalyst systems, including zeolite materials that can be operated without requirements for co-fed hydrogen.

09 BIOMASS FUELS↗
DOE OSTI2021

Identification of a pathway for electron uptake in Shewanella oneidensis

Extracellular electron transfer (EET) could enable electron uptake into microbial metabolism for the synthesis of complex, energy dense organic molecules from CO 2 and renewable electricity. Theoretically EET could do this with an efficiency comparable to H 2 -oxidation but without the need for a volatile intermediate and the problems it causes for scale up. However, significant gaps remain in understanding the mechanism and genetics of electron uptake. For example, studies of electron uptake in electroactive microbes have shown a role for the Mtr EET complex in the electroactive microbe Shewanella oneidensis MR-1, though there is substantial variation in the magnitude of effect deletion of these genes has depending on the terminal electron acceptor used. This speaks to the potential for previously uncharacterized and/or differentially utilized genes involved in electron uptake. To address this, we screened gene disruption mutants for 3667 genes, representing ≈99% of all nonessential genes, from the S. oneidensis whole genome knockout collection using a redox dye oxidation assay. Confirmation of electron uptake using electrochemical testing allowed us to identify five genes from S. oneidensis that are indispensable for electron uptake from a cathode. Knockout of each gene eliminates extracellular electron uptake, yet in four of the five cases produces no significant defect in electron donation to an anode. This result highlights both distinct electron uptake components and an electronic connection between aerobic and anaerobic electron transport chains that allow electrons from the reversible EET machinery to be coupled to different respiratory processes in S. oneidensis. Homologs to these genes across many different genera suggesting that electron uptake by EET coupled to respiration could be widespread. These gene discoveries provide a foundation for: studying this phenotype in exotic metal-oxidizing microbes, genetic optimization of electron uptake in S. oneidensis; and genetically engineering electron uptake into a highly tractable host like E. coli to complement recent advances in synthetic CO2 fixation.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2025

Ascorbic Acid Stability and pH Testing to Support RWM-018 Pilot Scale Wellhead Treatment System Feasibility Determination

A multitude of groundwater remediation techniques for chlorinated volatile organic compounds (cVOCs) have been conducted at the A/M-Areas of the Savannah River Site (SRS). Historical in-situ chemical oxidation (ISCO) injections of potassium permanganate and sodium persulfate conducted in 2018 and 2020, have left residual oxidant concentrations in the A/M-Area groundwater system. ISCO events targeted dense non-aqueous phase liquids (DNAPLs) through the injection of strong oxidants within plume zones upgradient of current groundwater recovery wells RWM-008 and RWM-018. These residual oxidants could significantly impede the operation of the mercury removal system needed to meet National Pollutant Discharge Elimination System (NPDES) permit requirements for the ongoing pump-and-treat system that hydraulically controls potions of the A/M-Area plume. Effluent treated groundwater from this system is discharged to surface water at the receiving outfall of the M-1 Air Stripper. To prevent interference of the M-1 Air Stripper system by residual oxidants, groundwater recovery has been ceased at well RWM-018. Modeling of oxidant transport in A/M-Area from ISCO estimated that the potential oxidant load contributed by RWM-018 could be as high as 120 mg/L. It is also possible that oxidants may be contributed via pumping at well RWM-008 in the near future as residual oxidants within the aquifer migrate toward its zone of influence. Savannah River National Laboratory (SRNL) has conducted research to investigate potential pre-treatment chemicals to neutralize these residual oxidants, before reaching the M-1 Air Stripper, to allow for resumed groundwater recovery at RWM-018 and continued pumping at RWM-008. Deployment of ascorbic acid for neutralization of residual oxidants at RWM-018 (and possibly RWM-008) is recommended based on results from previous reductant testing (SRNL, 2021). For a maximum estimated oxidant load at RWM-0018, a well-head treatment system would need to dose about 400 gallons of ascorbic acid each month to ensure complete neutralization. A second system with additional reagent should also be considered for deployment at RWM-008.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Material characterization of seven photovoltaic backsheets using seven accelerated test conditions

A variety of polymeric backsheet materials can be found in fielded photovoltaic (PV) modules, mostly based on fluoropolymer and polyethylene terephthalate (PET) materials. Cost reduction and sustainability considerations drive the recent development of alternative backsheet materials and designs [1]. In some fielded PV installations, polymeric materials are susceptible to environmental degradation in the form of backsheet cracking. To prevent backsheet degradation that can result in a module failure, thorough laboratory reliability testing is needed. In this report we studied the durability of seven commercial and experimental PV backsheets through accelerated stress testing using seven photolytic, hygrometric, and custom tests with the goal to understand if novel fluoropolymer-free backsheets are sufficiently environmentally durable to be commercialized. We divided the mechanisms observed during aging into two categories: core degradation and surface degradation. Although core degradation due to hydrolysis was observed in all commercial PET-, and polyamide (PA)-based backsheets aged with 85 degrees C/85% relative humidity, this test is unlikely to be field relevant. Photo-oxidative reactions on the exposed surface during UV weathering affected all seven backsheets regardless of the outer layer polymer material and additives. This degradation was limited to the outermost micrometers of the surface, except for backsheets containing PA-12, which resulted in surface cracking. A custom test combining UV with water spray caused the most severe backsheet degradation, including surface erosion and loss of insulating properties in polyolefin (PO)- and PA-based backsheets. This highlights the importance of combined accelerated stress testing to screen for complex backsheet degradation mechanisms. We also showed that, with material and design optimization, coextruded experimental PO-based backsheets have the potential to be a durable alternative to commercial PET- and fluoropolymer-based PV backsheets.

14 SOLAR ENERGY↗
DOE OSTI2024

Data and Scripts associated with “Lambda-PFLOTRAN: Workflow for Incorporating Organic Matter Chemistry Informed by Ultra High Resolution Mass Spectrometry into Biogeochemical Modeling.”

This data package is associated with the publication “Lambda-PFLOTRAN: Workflow for Incorporating Organic Matter Chemistry Informed by Ultra High Resolution Mass Spectrometry into Biogeochemical Modeling” submitted to Geoscientific Model Development (Muller et al., 2024). In this manuscript, organic matter chemistry and thermodynamics are directly connected to reactive transport simulators through the newly developed Lambda-PFLOTRAN (Parallel Reactive Flow and Transport model) workflow tool that succinctly incorporates organic matter chemistry data generated from Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS) into reaction networks to simulate aerobic respiration of the organic matter and the resulting biogeochemistry. Lambda-PFLOTRAN is a python-based workflow, executed through a Jupyter Notebook interface, that digests raw FTICR-MS data, develops a representative reaction network based on substrate-explicit thermodynamic modeling (also termed lambda modeling due to its key thermodynamic parameter λ used therein), and completes a biogeochemical simulation with the open source, reactive flow, and transport code PFLOTRAN. This data package contains Jupyter Notebook based workflows for two test cases for running biogeochemical simulations of organic matter oxidation identified by FTICR-MS. It contains four primary folders (workflow, data, src, and analysis), a file-level metadata file (Muller_2024_Lambda_PFLOTRAN_Manuscript_Data_Package_flmd.csv) that lists all the files contained in this data package with a short description of each, and a data dictionary (Muller_2024_Lambda_PFLOTRAN_Manuscript_Data_Package_dd.csv) file that describes the tabular column headers. The ‘workflow’ folder contains the Jupyter Notebook based workflows for running the lambda analysis, PFLOTRAN simulation, sensitivity analysis and parameter estimation. The ‘data’ folder contains the FTICR-MS data, initial conditions, and incubation data for test cases 1 and 2 in folders titled ‘WHONDRS’ and ‘Colloids’, respectively. The data folder also has a ‘Database’ folder containing a reaction network for bulk organic matter (assumed to be CH2O) and a general database for PFLOTRAN (hanford_rxn_network). The CH2O reaction network defines bulk organic matter oxidation. Biogeochemical simulations are completed for both the lambda binned organic matter and bulk organic matter reaction networks. The ‘hanford_rxn_network’ database includes information required for PFLTORAN simulations including ion size, molar mass, and charge of the aqueous species, gases, and minerals phases. The ‘src’ folder contains python source codes for performing lambda analysis, PFLOTRAN simulation, sensitivity analysis and parameter estimation. The ‘analysis’ folder contains outputs from the test cases 1 and 2 including lambda analysis, PFLOTRAN runs and the calibration results.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Redistribution of Ru in Fe 2 O 3 –Ru Nanocatalysts through an Oxidative Pretreatment Improves Reverse Water–Gas Shift Activity

We have synthesized Fe–Ru nanoparticles via a solvothermal method to create catalysts for the reverse water–gas shift reaction and demonstrated the impact of reductive and oxidative pretreatments on both catalytic performance and structure. Catalytic testing showed improved activity after exposure to O 2 at 600 °C. In contrast, the activity became lower if then exposed to H 2 at 600 °C. Environmental scanning transmission electron microscopy and scanning electron microscopy showed that exposure to O 2 at 600 °C changes the morphology and completely oxidizes Fe into Fe 2 O 3 . Exposure to H 2 at elevated temperature caused Ru coalescence at the surface of the nanoparticle, forming clusters which decreased the optimization of Ru. Reoxidation of the particles exposed to H 2 , however, caused a redistribution of Ru that appears beneficial in maximizing Ru exposure and synergy with Fe oxide, with no major changes in the morphology and oxide structure. Furthermore, our diagnostics demonstrate the complex and reversible rearrangements possible in these multicomponent particles and the benefits of oxidative pretreatment to enhance or regenerate Fe–Ru catalysts in other important catalytic reactions such as Fischer–Tropsch synthesis.

Fe−Ru nanoparticles↗
DOE OSTI2021

Investigation of breakaway corrosion observed during oxide growth in pure and low alloying element content Zr exposed in water at 360°C

The addition of small concentrations of alloying elements to pure zirconium can prevent nuclear fuel cladding material from undergoing unstable oxide growth in aqueous environments at light water reactor operating temperatures. The role of alloying elements in stabilizing the oxide growth is examined in this paper, to better understand the oxide growth stabilization mechanism. To this end, a set of initial, short-duration corrosion experiments were performed, followed by oxide layer characterization. Specifically, ten model Zr alloys were selected to test the effect of small alloying additions on the alloy corrosion rate and corrosion breakaway. Additionally, these alloys were corrosion tested in pure water in an autoclave at 360°C for up to 70 days. The alloys included crystal bar Zr, sponge Zr, and model alloys with small concentrations of Sn, Fe, and Cr. After testing, the alloys were characterized using scanning electron microscopy (SEM) and synchrotron µ-X-ray fluorescence (µXRF) to study how the structure of the oxide and alloying element distribution related to unstable oxide growth. Initial results in the 360°C water environment showed breakaway oxidation may be caused by unstable oxide growth due to heterogeneous distribution of the alloying elements. Heterogeneous distribution of alloying elements was correlated to the occurrence of unstable oxide growth (either nodule-like, grain boundary penetration, or differential grain-to-grain growth). It is possible that this heterogeneity, made possible by low alloying element content, can cause breakaway corrosion, but further study is warranted.

36 MATERIALS SCIENCE↗
DOE OSTI2022

MPCVD-Grown Nanodiamond Microelectrodes with Oxygen Plasma Activation for Neurochemical Applications

Nanodiamonds (NDs) are a carbon nanomaterial that has a diamond core with heteroatoms and defects at the surface. The large surface area, defect sites, and functional groups on NDs make them a promising material for electrochemical sensing. Previously, we dip-coated ND onto carbon-fiber microelectrodes (CFMEs) and found increases in sensitivity, but the coating was sparse. Here, for this work, we directly grew thin films of ND on niobium wires using microwave plasma chemical vapor deposition (MP-CVD) to provide full surface coverage. ND microelectrodes show a reliable performance in neurotransmitter detection with good antifouling properties. To improve sensitivity, we oxygen plasma etched ND films to activate the surface and intentionally add defects and oxygen surface functional groups. For fast-scan cyclic voltammetry detection of dopamine, oxygen plasma-etching increases the sensitivity from 21 nA/μM to 90 nA/μM after treatment. Fouling was tested by repeated injections of serotonin or tyramine, and both ND and plasma oxidized nanodiamond (NDO) microelectrodes maintain their currents better compared to CFMEs and therefore are more antifouling. Furthermore, a biofouling test in brain slices shows that ND microelectrodes barely have any current drop, while the more hydrophilic NDO microelectrodes decrease more, but still not as much as CFMEs. Overall, grown ND microelectrodes are promising in neurotransmitter detection with excellent fouling resistance, whereas oxygen plasma etching slightly lowers the fouling resistance but dramatically increases sensitivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Influence of thermal treatment on structure and catalytic performance of ceria-zirconia supported copper oxide (CuO x /Ce y Zr 1-y O 2 ) catalysts for CO oxidation

Copper oxide (CuO x ) supported on ceria-zirconia (Ce y Zr 1-y O 2 , y = 1.0, 0.5, 0.0) catalysts were investigated to elucidate the effects of thermal treatment on their physicochemical properties and catalytic performance in carbon monoxide (CO) oxidation. Here, the catalysts were synthesized via a one-pot chemical vapor deposition (OP-CVD) method at 700˚C and 900˚C with controlled Cu loading. Characterization techniques, including synchrotron X-ray diffraction (S-XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma spectroscopy (ICP), and N 2 adsorption-desorption, were implemented to probe the crystalline structure, molecular and electronic structure, oxygen vacancies, specific surface area (SSA) and metal loading. CO oxidation was chosen as a model reaction to explore the structure-catalytic performance relationship. A ∼100% CO conversion was achieved at < 150˚C, particularly with the CuO x /CeO 2 catalyst calcined at 700˚C. In contrast, calcination at 900˚C caused a ∼90% decrease in SSA and a ∼24% increase in T 50 . Activity tests revealed that increasing ZrO 2 content lowered CO oxidation activity despite generating more defect sites. In-situ measurement of the 700 °C calcined samples revealed the presence of stable and unstable defects in CuO x /Ce 0.5 Zr 0.5 O 2 and CeO 2 respectively, which play a key role in the activity of the catalysts. The results highlight that catalytic performance is closely related to the SSA. Furthermore, an optimum calcination temperature favor significant oxygen vacancy formation with required CuO x -support interactions, enhancing redox properties and catalytic performance.

36 MATERIALS SCIENCE↗
DOE OSTI2026

The Explosive Hazards of Icosahedral Carboranes and Dodecaborate with Common Oxidizers and Salts

Carboranes find use in a wide variety of applications ranging from specialty catalysts to medicinal uses. Certain functionalized carboranes are described as explosive materials, although their nonfunctionalized precursors are regarded as inherently stable and not explosive. Herein, we report new findings on the sensitization of nonfunctionalized 12-vertex ortho-, meta-, and para-carboranes as well as dodecaborate in physical mixtures with several common inorganic salts. These mixtures were evaluated for explosive properties with drop hammer impact tests, friction tests, and differential scanning calorimetry thermal gravimetric analysis (DSC-TGA). Results indicate explosive sensitization to mechanical stimuli for the nonfunctionalized carboranes tested with a wide variety of inorganic salts, especially oxidizers. Sensitization of these compounds has not previously been reported, and raising awareness to the broader scientific community on this matter is warranted, especially as several of the mixtures evaluated are more sensitive to mechanical stimuli than primary explosives such as lead azide or pentaerythritol tetranitrate.

36 MATERIALS SCIENCE↗
DOE OSTI2023

SPC-3178 Rev 5 Beryllium Oxide Procurement Specification

TREAT microreactor Experiment Cell (T-REXC). This facility will provide a test bed for microreactor developers to perform demonstration projects and critical experiments in an expedited manner. In addition to other systems, structures, and components (SSCs), T-REXC will provide beryllium oxide (BeO) reflector components that T-REXC users can incorporate into their equipment installation. This specification details supplier requirements associated with these BeO components.

21 - SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLAN↗