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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 217 records · Page 12
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Catalyzed oxidation of IG-110 nuclear graphite by simulated fission products Ag and Pd nanoparticles

To evaluate the stability of nuclear materials in high temperature gas reactors under air ingress conditions, catalytic oxidation of IG-110 graphite by two simulated fission products, metallic Pd and Ag, was studied in oxidative atmosphere and at temperatures up to 1000°C using an integrated furnace, mass spectroscopy and infrared spectroscopy system. Transmission electron microscopy and X-ray diffraction studies show that Pd and Ag nanoparticles were successfully introduced onto powdery IG-110 graphite through an impregnation and subsequent heat-treatment process. The combined mass spectroscopy and infrared spectroscopy methods allow simultaneous analysis of two gaseous products, CO and CO 2 , and separate measurements of activation energy for their formation reactions. It was found that the introduction of Pd or Ag to IG-110 graphite substantially catalyzed the oxidation of graphite, characteristic of decreased onset temperatures for the oxidation of graphite. Moreover, the catalytic effects by Pd and Ag are considerably different based on measured concentration ratios of CO 2 to CO as a function of oxidation temperatures. Ag makes the graphite oxidation commence at approximately 400°C with CO 2 being the dominant product. In contrast, Pd significantly increases the concentration ratio of CO 2 to CO at temperatures higher than approximately 690°C, although it decreases the onset temperature for the oxidation reaction to around 525°C. To understand the catalytic difference, the mechanism of the graphite oxidation was discussed based on the changes of surface oxygen species on Ag and Pd.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

Ultrasmall Cu Nanoparticles Supported on Crystalline, Mesoporous ZnO for Selective CO 2 Hydrogenation

Converting CO 2 to value-added chemicals, e. g., CH 3 OH, is highly desirable in terms of the carbon cycling while reducing CO 2 emission from fossil fuel combustion. Cu-based nanocatalysts are among the most efficient for selective CO 2 -to-CH 3 OH transformation; this conversion, however, suffers from low reactivity especially in the thermodynamically favored low temperature range. We herein report ultrasmall copper (Cu) nanocatalysts supported on crystalline, mesoporous zinc oxide nanoplate (Cu@mZnO) with notable activity and selectivity of CO 2 -to-CH 3 OH in the low temperature range of 200–250 °C. Cu@mZnO nanoplates are prepared based on the crystal-crystal transition of mixed Cu and Zn basic carbonates to mesoporous metal oxides and subsequent hydrogen reduction. Under the nanoconfinement of mesopores in crystalline ZnO frameworks, ultrasmall Cu nanoparticles with an average diameter of 2.5 nm are produced. Cu@mZnO catalysts have a peak CH 3 OH formation rate of 1.13 mol h −1 per 1 kg under ambient pressure at 246 °C, about 25 °C lower as compared to that of the benchmark catalyst of Cu−Zn−Al oxides. In conclusion, our new synthetic strategy sheds some valuable insights into the design of porous catalysts for the important conversion of CO 2 -to-CH 3 OH.

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

CeO2 Nanoparticle Doping as a Probe of Active Site Speciation in the Catalytic Hydrolysis of Organophosphates

Organophosphate hydrolysis is important for degrading environmentally harmful compounds and recovering phosphate ions in biological molecules. CeO2 nanocrystals have been well-studied for dephosphorylation via hydrolysis owing to the accessible and tunable distribution of Ce3+ and Ce4+ ions. However, there remains uncertainty in the literature regarding which surface defect properties direct catalytic activity, such as the Ce3+/Ce4+ distribution, oxygen vacancies, faceting, and dopants, and to what degree they contribute to efficient hydrolysis. Trivalent (M3+) dopants serve as a tool for manipulating defects, including the concentration of Ce3+ and oxygen vacancies, thereby influencing the hydrolytic activity of CeO2. Herein, trivalent metal ions (M = Y3+, Cr3+, In3+, and Gd3+) were employed to modulate the active sites on the CeO2 nanocrystal surface, and the effects of each metal dopant on the cerium oxide active sites for organophosphate hydrolysis were investigated. M-doped CeO2 nanoparticles were synthesized via hydrothermal methods, followed by annealing to remove ligands and prime the nanocrystal surface for catalysis. Catalytic performance was evaluated using dimethyl-p¬-nitrophenyl phosphate (DMNP) as a model organophosphate substrate, with degradation monitored over time using UV-visible absorption spectroscopy. Powder X-ray diffraction (PXRD), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy revealed successful doping of CeO2 in all cases, albeit with distinctive characteristics demonstrating how M3+ dopants affect catalysis. We show that CeO2 exhibits high sensitivity to dopants that generate lattice strain, Ce3+ ions, and oxygen vacancy defects. Consequently, achieving high catalytic efficiency within CeO2 requires a balanced active site ensemble, wherein defects are maintained at optimal concentrations and distributions on the nanocrystal surface.

Miura-Stempel, Emily L.↗
DOE OSTI2022

A single-Pt-atom-on-Ru-nanoparticle electrocatalyst for CO-resilient methanol oxidation

Single Pt atom catalysts are key targets because a high exposure of Pt substantially enhances electrocatalytic activity. In addition, PtRu alloy nanoparticles are the most active catalysts for the methanol oxidation reaction. To combine the exceptional activity of single Pt atom catalysts with an active Ru support we must overcome the synthetic challenge of forming single Pt atoms on noble metal nanoparticles. In this report we demonstrate a process that grows and spreads Pt islands on Ru branched nanoparticles to create single-Pt-atom-on-Ru catalysts. By following the spreading process by in situ TEM, we found that the formation of a stable single atom structure is thermodynamically driven by the formation of strong Pt–Ru bonds and the lowering of the surface energy of the Pt islands. The stability of the single-Pt-atom-on-Ru structure and its resilience to CO poisoning result in a high current density and mass activity for the methanol oxidation reaction over time.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Visualizing Size-Dependent Dynamics of CeO 2-δ {100}-Supported CoO x Nanoparticles Under CO 2 Hydrogenation Conditions

Carbon dioxide is a major greenhouse gas. In order to optimize processes focused on its chemical valorization, one needs detailed information about the effects of CO 2 and/or CO 2 /H 2 mixtures on the structure and morphology of metal/oxide catalysts. Here, in this study, the evolution of a catalyst with cobalt supported on CeO 2 -cube nanostructures under CO 2 hydrogenation conditions was investigated by using a set of in situ characterization techniques (X-ray absorption fine structure, X-ray diffraction, diffuse reflectance infrared Fourier transform spectroscopy, and environmental transmission electron microscopy (TEM)). The {100} facets of the ceria support displayed an unexpectedly high stability due to strong interactions with the aggregates of cobalt oxide. A significant influence of interfacial bonding between CoO x and CeO 2-δ {100} is evident through a clear preference in the orientation of CoO x nanoparticles (NPs) with respect to the substrate. For initially reduced Co/CeO 2 -cube nanostructures, a kinetically controlled oxidation of cobalt upon the introduction of CO 2 was observed during the early stages of CO 2 hydrogenation. Environmental TEM revealed the size-dependent morphological behavior of cobalt oxide NPs due to strong interactions with the CeO 2 {100} surface. When the environment was switched from H 2 to a mixture of H 2 and CO 2 at 250 °C, small CoO x NPs (in the largest dimension < 2.5 nm) rapidly transformed from a pyramidal three-dimensional (3D) form to a planar, monatomic layer attached to the concurrently oxidized CeO 2-δ {100} surface. This maximizes the number of sites available for the binding of CO 2 or reaction intermediates. The shape transformation reflected the oxophilic character of cobalt and strong metal–support interactions. The removal of CO 2 from the gas phase led to a reduction of the cobalt oxide NPs by hydrogen and a reversible two-dimensional → 3D transformation. In contrast, no significant morphological changes, apart from further oxidation, were observed for big CoO x NPs (in the largest dimension > 3 nm). These trends are not seen for nanoparticles of noble metals. The observed morphological and structural changes in the small CoO x NPs affected the stability of reaction intermediates and modified the selectivity of the CoO x /CeO 2 catalyst system for methane production.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Multivariate Bayesian Optimization of CoO Nanoparticles for CO 2 Hydrogenation Catalysis

The hydrogenation of CO 2 holds promise for transforming the production of renewable fuels and chemicals. However, the challenge lies in developing robust and selective catalysts for this process. Transition metal oxide catalysts, particularly cobalt oxide, have shown potential for CO 2 hydrogenation, with performance heavily reliant on crystal phase and morphology. Achieving precise control over these catalyst attributes through colloidal nanoparticle synthesis could pave the way for catalyst and process advancement. Yet, navigating the complexities of colloidal nanoparticle syntheses, governed by numerous input variables, poses a significant challenge in systematically controlling resultant catalyst features. We present a multivariate Bayesian optimization, coupled with a data-driven classifier, to map the synthetic design space for colloidal CoO nanoparticles and simultaneously optimize them for multiple catalytically relevant features within a target crystalline phase. The optimized experimental conditions yielded small, phase-pure rock salt CoO nanoparticles of uniform size and shape. These optimized nanoparticles were then supported on SiO 2 and assessed for thermocatalytic CO 2 hydrogenation against larger, polydisperse CoO nanoparticles on SiO 2 and a conventionally prepared catalyst. The optimized CoO/SiO 2 catalyst consistently exhibited higher activity and CH 4 selectivity (ca. 98%) across various pretreatment reduction temperatures as compared to the other catalysts. This remarkable performance was attributed to particle stability and consistent H* surface coverage, even after undergoing the highest temperature reduction, achieving a more stable catalytic species that resists sintering and carbon occlusion.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2003

Synthesis of substantially monodispersed colloids

A method of forming ligated nanoparticles of the formula Y(Z).sub.x where Y is a nanoparticle selected from the group consisting of elemental metals having atomic numbers ranging from 21-34, 39-52, 57-83 and 89-102, all inclusive, the halides, oxides and sulfides of such metals, and the alkali metal and alkaline earth metal halides, and Z represents ligand moieties such as the alkyl thiols. In the method, a first colloidal dispersion is formed made up of nanoparticles solvated in a molar excess of a first solvent (preferably a ketone such as acetone), a second solvent different than the first solvent (preferably an organic aryl solvent such as toluene) and a quantity of ligand moieties; the first solvent is then removed under vacuum and the ligand moieties ligate to the nanoparticles to give a second colloidal dispersion of the ligated nanoparticles solvated in the second solvent. If substantially monodispersed nanoparticles are desired, the second dispersion is subjected to a digestive ripening process. Upon drying, the ligated nanoparticles may form a three-dimensional superlattice structure.

Klabunde, Kenneth J.↗
DOE OSTI2023

Metal–Organic Framework as a New Type of Magnetothermally‐Triggered On‐Demand Release Carrier

The development of external stimuli‐controlled payload systems has been sought after with increasing interest toward magnetothermally‐triggered drug release (MTDR) carriers due to their non‐invasive features. However, current MTDR carriers present several limitations, such as poor heating efficiency caused by the aggregation of iron oxide nanoparticles (IONPs) or the presence of antiferromagnetic phases which affect their efficiency. Herein, a novel MTDR carrier is developed using a controlled encapsulation method that fully fixes and confines IONPs of various sizes within the metal–organic frameworks (MOFs). This novel carrier preserves the MOF's morphology, porosity, and IONP segregation, while enhances heating efficiency through the oxidation of antiferromagnetic phases in IONPs during encapsulation. It also features a magnetothermally‐responsive nanobrush that is stimulated by an alternating magnetic field to enable on‐demand drug release. The novel carrier shows improved heating, which has potential applications as contrast agents and for combined chemo and magnetic hyperthermia therapy. It holds a great promise for magneto‐thermally modulated drug dosing at tumor sites, making it an exciting avenue for cancer treatment.

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

Strain‐Enhanced Metallic Intermixing in Shape‐Controlled Multilayered Core–Shell Nanostructures: Toward Shaped Intermetallics

Abstract Controlling the surface composition of shaped bimetallic nanoparticles could offer precise tunability of geometric and electronic surface structure for new nanocatalysts. To achieve this goal, a platform for studying the intermixing process in a shaped nanoparticle was designed, using multilayered Pd‐Ni‐Pt core–shell nanocubes as precursors. Under mild conditions, the intermixing between Ni and Pt could be tuned by changing layer thickness and number, triggering intermixing while preserving nanoparticle shape. Intermixing of the two metals is monitored using transmission electron microscopy. The surface structure evolution is characterized using electrochemical methanol oxidation. DFT calculations suggest that the low‐temperature mixing is enhanced by shorter diffusion lengths and strain introduced by the layered structure. The platform and insights presented are an advance toward the realization of shape‐controlled multimetallic nanoparticles tailored to each potential application.

Williams, Benjamin P.↗
DOE OSTI2021

Bismuth-Functionalized Silica Aerogels for Iodine Capture

The U.S. Department of Energy is looking into alternative sorbents for the removal of radioiodine from off-gas streams in a used nuclear fuel reprocessing plant. One class of sorbents considered are bismuth-functionalized silica aerogels which offer an efficient capture of iodine from off-gas streams and are environmentally friendly and lower cost when compared to silver-functionalized sorbents. Two types of bismuth-functionalized silica aerogels were successfully manufactured using a hierarchical synthesis approach:1) The Bi 3+ -aerogel with bismuth oxide nitrate hydroxide hydrate particles and 2) Bi-aerogel with bismuth metal and bismuth sulfide nanoparticles. Both sorbents exhibited high sorption capacity for iodine. However, presence of particles of different composition, size, and distribution on aerogel support resulted in different iodine loadings. The Bi 3+ -aerogel exhibited sorption capacity of 289 mg/g. In contrast, Bi-aerogel exhibited more that 20% higher sorption capacity. The heat-treatment of Bi 3+ -aerogel at 225? under hydrogen atmosphere increased iodine loading capacity to 351 mg/g.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRSDate not supplied

Quick and Correlative TOF-SIMS Analysis of Dispersoid Content in Powder Feedstock and Printed Oxide Dispersion Strengthened Alloys

Oxide dispersion strengthening (ODS) of metal alloys, when combined with additive manufacturing (AM), can be used to solve high-temperature material application problems. The performance of ODS materials is dependent on nano-scale oxide being distributed uniformly throughout the metal matrix; a homogenous distribution is critical to the creep and yield strength. Therefore, quantifying and analyzing these oxide nanoparticles is essential for ODS alloy development. Assessing the chemistry and morphology of dispersoids in a material can be conducted using a variety of X-ray and electron-based methods. Time of Flight Secondary Ion Mass Spectrometry (TOF-SIMS), which assesses chemical concentrations from ion masses, provides the necessary spatial resolution and avoids potential spectral overlap of all elements present. In this work, preparing ODS powder feedstock and Laser Powder Bed Fusion AM was conducted with a NiCoCr alloy and yttria dispersoid, mixed with a Resodyn resonance mixer and printed on an EOS M100 3D printer at NASA Glenn. TOF-SIMS was performed on a Physical Electronics NanoTOF TRIFT V TOF-SIMS at Case Western Reserve University. The TOF-SIMS results collected on the feedstock powder samples correspond to the qualitative interpretation of the homogeneity of the oxide coating on the metal powder from SEM images. This provides quantitative support to the qualitative microscopy images collected earlier in the process design phase. The variance in the yttrium distribution on the powder feedstock samples also correlated with the variance of the yttrium distribution detected in the printed samples. This correlation supported the hypothesis that an even coating of yttria on the metal powders contributes to an even distribution of yttria in the printed material.

Laura G. Wilson↗
DOE OSTI2021

Predicting a Key Catalyst-Performance Descriptor for Supported Metal Nanoparticles: Metal Chemical Potential

The chemical potential of metal atoms in supported nanoparticles provides a convenient descriptor of their performance as heterogeneous catalysts that captures the effects of particle size, support and alloying. Based on microcalorimetric measurements, the chemical potential is shown in this work to be predictable as a function of monometallic particle diameter and the adhesion energy of the particle to the support, and, for oxide supports, this adhesion energy correlates predictably with metal oxophilicity. These correlations provide predictions of metal chemical potential that can enable catalyst design. They also suggest an improvement in the Gibbs-Thomson relation for free-standing nanoparticles, whether metals or molecular solids.

metal/oxide interface↗
DOE OSTI2022

Higher loadings of Pt single atoms and clusters over reducible metal oxides: application to C–O bond activation

We develop higher loadings of isolated noble metal atoms and clusters on a mildly reducible metal oxide. Here we demonstrate the approach for Pt supported on TiO 2 and confirmed it by XRD, AC-HAADF-STEM, CO-FTIR, XAS, and XPS. Density functional theory calculations rationalize the experimental stability and the IR shifts using mixtures of CH 3 I and CO. The redispersed catalysts are thermally stable in inert gas or H 2 and afford enhanced selectivity and activity in hydrodeoxygenation reactions compared to metal nanoparticles by creating surface oxygen vacancies that promote C–O cleavage without side reactions. Higher metal loadings, e.g., 1%Pt/TiO 2 , on the oxide surface profoundly increase the activity of the bare oxide catalyst tenfold compared to ultra-low loadings typically used for single atom catalysis.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Controlling Heterogeneous Catalysis with Organic Monolayers on Metal Oxides

A key theme of heterogeneous catalysis research is achieving control of the environment surrounding the active site to precisely steer the reactivity toward desired reaction products. One method toward this goal has been the use of organic ligands or self-assembled monolayers (SAMs) on metal nanoparticles. Metal-bound SAMs are typically employed to improve catalyst selectivity but often decrease the reaction rate as a result of site blocking from the ligands. Recently, the use of metal oxide-bound organic modifiers such as organophosphonic acid (PA) SAMs has shown promise as an additional method for tuning reactions on metal oxide surfaces as well as modifying oxide-supported metal catalysts. In this Account, we summarize recent approaches to enhance catalyst performance with oxide-bound monolayers. These approaches include (1) modification of metal oxide catalysts to tune surface reactions, (2) formation of SAMs on the oxide component of supported metal catalysts to modify sites at the metal–support interface, and (3) enhancement of catalyst performance (e.g., stability) through modification of sites remote from the active sites. Further, both the headgroups and organic tail groups of PA SAMs or other ligands can influence reactions on metal oxide surfaces. Binding of the headgroup can selectively poison certain active sites, altering the selectivity in a manner analogous to metal-bound ligands (at the expense of active site quantity). Moreover, tail groups can be functionalized to interact favorably with reactants and intermediates, for instance through dipole–dipole interactions. On supported metal catalysts like Pt/Al 2 O 3 , PA SAMs can selectively form on the oxide support. This selective deposition allows for modification of the metal–support interface with minimal blockage of metal sites. PA headgroups were shown to provide tunable acid sites at the interface, dramatically improving hydrodeoxygenation rates of various alcohols. Additionally, organic tail functionality was used to activate or stabilize specific reactants at the interface, such as with the use of amine-functionalized PAs to stabilize chemisorption of CO 2 during the reverse water gas shift reaction. PAs have also been found to affect the electronic properties of bulk metal sites through long-range electron withdrawal via the oxide, providing an additional avenue to tune catalytic behavior. Finally, organic modifiers were shown to enhance catalytic performance without directly modifying the active site. For instance, in biphasic liquid environments the modification of catalyst particles with hydrophobic or hydrophilic SAMs shifts the selectivity of multipath reactions on the basis of the hydrophobicities of different intermediates and products. As another “long-range” effect, the deposition of ligands on oxide supports improved catalyst stability through both improved resistance to sintering and suppression of active site poisoning. The recent contributions discussed in this Account demonstrate the versatility and significant potential for the approach of modifying catalysts with oxide-bound organic monolayers.

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

The Impact of Catalyst Layer Composition and Structure on Performance and Durability of PEMWE Anodes

A study of various compositions of anodes for proton exchange membrane water electrolysis aimed at reducing precious metal content and system costs without compromising performance and durability is presented. A key challenge in current water electrolysis technologies is the reliance on high iridium loadings to ensure sufficient catalytic activity, electronic conductivity, and durability for the oxygen evolution reaction. To address this, catalyst layers based on the stable but kinetically limited rutile phase of iridium oxide are combined with platinum nanoparticles and carbon-based additives to improve structural properties and ink processability. By systematically varying the volume ratios of carbon to precious metals and ionomer to solids, compositional trends have been identified, and significant performance improvements have been achieved. Structural and elemental analysis confirms improved dispersion of platinum and iridium can be achieved, as well as electronic conductivity improvements within the catalyst layer. Polarization curve analysis has shown the ability of added Pt and C to significantly increase catalytic activity. These results highlight the potential positive impact of Pt and C on anode structure, composition, and cell performance.

36 MATERIALS SCIENCE↗
NASA NTRS2009

Synthesis Methods, Microscopy Characterization and Device Integration of Nanoscale Metal Oxide Semiconductors for Gas Sensing in Aerospace Applications

A comparison is made between SnO2, ZnO, and TiO2 single-crystal nanowires and SnO2 polycrystalline nanofibers for gas sensing. Both nanostructures possess a one-dimensional morphology. Different synthesis methods are used to produce these materials: thermal evaporation-condensation (TEC), controlled oxidation, and electrospinning. Advantages and limitations of each technique are listed. Practical issues associated with harvesting, purification, and integration of these materials into sensing devices are detailed. For comparison to the nascent form, these sensing materials are surface coated with Pd and Pt nanoparticles. Gas sensing tests, with respect to H2, are conducted at ambient and elevated temperatures. Comparative normalized responses and time constants for the catalyst and noncatalyst systems provide a basis for identification of the superior metal-oxide nanostructure and catalyst combination. With temperature-dependent data, Arrhenius analyses are made to determine an activation energy for the catalyst-assisted systems.

VanderWal, Randy L.↗
DOE OSTI2025

Constructing Highly Durable Fuel Cell Catalysts Through Integrating Graphitic Shell‐Protected Composite Carbon Support with Gaseous Co Deposition‐Driven PtCo Intermetallics

Metal dissolution, nanoparticle agglomeration, and carbon support corrosion cause significant performance degradation of current PtCo catalysts under acidic and oxidative oxygen reduction reaction. Here, in this study, an integrated strategy is presented to design high-performance Pt 3 Co intermetallic catalysts by regulating gaseous Co deposition-driven diffusion into Pt nanoparticles supported on a composite carbon. The composite carbon is derived from ZIF-8/polyaniline, consisting of a high-surface-area (HSC) core and a protective graphitic shell (GS), which is employed to design 40 wt.% Pt/HSC@GS catalyst. The corresponding membrane electrode assemblies (MEAs) can maintain 1.09 A cm −2 at 0.7 V (20. 7% loss) after 10 000 cycles (1.0–1.5 V for carbon stability) and 1.15 A cm −2 (16.1% loss) after 150 000 cycles (0.60–0.95 V for catalyst stability). A ordered Pt 3 Co intermetallic is synthesized via a gaseous Co-deposition process, which yields a homogeneous Co-rich layer onto the Pt nanoparticles on the composite support, thereby facilitating Co diffusion into Pt crystal during subsequent ordering annealing to form the ordered intermetallic structure. This gaseous deposition leads to a thin carbon layer on PtCo nanoparticles, inhibiting particle growth during the annealing and mitigating Co dissolution under dynamic electrochemical conditions. The PtCo catalyst achieves impressive MEA performance and long-term durability (1.45 A cm −2 at 0.7 V after 120 000 cycles) under heavy-duty conditions.

30 DIRECT ENERGY CONVERSION↗
NASA NTRS2005

Cobalt Oxide Hollow Nanoparticles Derived by Bio-Templating

We present here the first fabrication of hollow cobalt oxide nanoparticles produced by a protein-regulated site-specific reconstitution process in aqueous solution and describe the metal growth mechanism in the ferritin interior.

Kim, Jae-Woo↗