Search NASA⌕ Search

SEARCH · Search NASA

Results for “Complex metal oxide”

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 163 records · Page 9

Surface immobilized copper(i) diimine photosensitizers as molecular probes for elucidating the effects of confinement at interfaces for solar energy conversion

Heteroleptic copper(I) bis(phenanthroline) complexes with surface anchoring carboxylate groups have been synthesized and immobilized on nanoporous metal oxide substrates. The species investigated are responsive to the external environment and this work provides a new strategy to control charge transfer processes for efficient solar energy conversion.

14 SOLAR ENERGY↗

Plutonium Oxidation State Distribution in the Presence of WIPP-Relevant Organics and Iron Corrosion Products

The oxidation state and solubility of plutonium (Pu) in high ionic strength synthetic WIPP (Waste Isolation Pilot Plant) brines as a function of pC H+ in the presence and absence of WIPP-relevant organic ligands (EDTA [Ethylenediaminetetraacetic acid], oxalate, citrate, acetate) and iron corrosion products (magnetite and metallic iron) at 𝑇 = 23 ± 2 ∘C was thoroughly studied by long-term batch solubility experiments (between approximately 800-1,100 days) from an undersaturation approach. The oxidation state of Pu in the WIPP environment has been a topic of interest since the initial Compliance Certification Application (CCA). This study aims to investigate the solubility of Pu under the expected WIPP conditions and to determine the oxidation state of the solid phase that will control the solubility. One of the most important results of this study is that the Pu oxidation state was analyzed both from the surface area of the corrosion products and in the precipitated solid. The analysis of the Pu oxidation state on the surface of the iron mineral from the ongoing undersaturated experiments is more relevant to the performance assessment of nuclear waste disposal than short term batch (plutonium-iron phase) experiments. The X-ray Absorption Near-Edge Spectroscopy (XANES) analysis showed that Pu oxidation state is different on the metal surface and in the precipitated solid. Pu(III) is the dominant oxidation state in the metallic iron (Fe 0 ) system in the presence and absence of organics. Pu(IV) is the dominant oxidation state in the magnetite system in the presence and absence of organics. Also, organics stabilize Pu(IV) in the magnetite system. Analysis of Pu in the precipitated solid by Extended X-ray Absorption Fine Structure (EXAFS) analysis showed that Pu formed an inner-sphere complex with iron with minor amounts of PuO 2 present. X-ray diffraction (XRD) results indicate that metallic iron and magnetite did not oxidize in three years in the alkaline and high ionic strength system. Under these conditions (8 < pC H+ < 10 at T = (22 ± 2) °C under nitrogen atmosphere, the solubility of Pu changes by up to three orders of magnitude (10 -5 and 10 -8 M). The spread in solubility is highest at pC H+ = 9. Pu(III) and Pu(IV) showed different solubility behavior in the synthetic WIPP brine. A summary of the data collected in this report will be submitted to Sandia National Laboratories as part of a parameter update report which will outline the changes to the OXSTAT parameter for the 2026 Compliance Recertification Application (CRA-2026). The experiments performed were done according to the U.S. Department of Energy (DOE) approved Test Plan entitled “Effects of Radiolysis, Organic Complexation, and Redox Conditions on the Speciation and Oxidation State Distribution of Pu(III/IV)” (LCO-ACP-25). All data reported were obtained under the Los Alamos National Laboratory-Carlsbad Office (LANL-CO) Quality Assurance Program, which is compliant with the DOE Carlsbad Field Office, Quality Assurance Program Document (CBFO/QAPD).

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Homogeneous Gold Redox Chemistry: Organometallics, Catalysis, and Beyond

Gold redox chemistry holds the promise of unique reactivities and selectivities that are different to other transition metals. Recent studies have utilized strain release, ligand design, and photochemistry to promote the otherwise sluggish oxidative addition to Au(I) complexes. More details on the reductive elimination from Au(III) complexes have also been revealed. These discoveries have facilitated the development of gold redox catalysis and will continue to offer mechanistic insight and inspiration for other transition metals. Furthermore, this review highlights how research in organometallic chemistry has led to gold redox catalysis, as well as applications in materials science, bioconjugation, and radiochemical synthesis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Air oxidation of yttrium hydride as a high temperature moderator for thermal neutron spectrum fission reactors

Yttrium hydride (YH x ) is an attractive moderator material for thermal neutron spectrum fission reactors requiring a small reactor core volume and has been selected as the neutron moderator for the Transformational Challenge Reactor (TCR), an advanced gas-cooled microreactor. Before YH x can be used in this application, it is important to understand the material response to off-normal conditions. In the present study, 550–650 °C isothermal dry air oxidation was performed to simulate a depressurized loss of force circulation (DLOFC) event. The oxidation was performed using thermogravimetric analysis (TGA) on bulk crack-free YHx coupons. Oxidation studies were also performed on Y coupons to elucidate the impact of H on oxidation. Both the chemistry and distribution of processing impurities were found to strongly affect oxidization behavior on a batch-to-batch basis. Regardless of batch, YHx oxidized at a significantly lower rate than Y at all temperatures, and the lower rate was directly correlated with increased hydride content. Metallic Y exhibited complex exponential kinetics, whereas YH x also exhibited complex kinetics but gained considerably less mass. According to literature reports on protonic and native-ion conductivities of Y 2 O 3 and mass spectrometry analysis of gaseous reaction products formed during the oxidation of YH x , a mechanism for the reduced oxidation rate of yttrium hydride is suggested.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Design of Efficient Molecular Electrocatalysts for Water and Carbon Dioxide Reduction Using Predictive Models of Thermodynamic Properties

Objectives: 1) To design and synthesize water soluble transition metal complexes that function as electrocatalysts for the reduction of water to hydrogen or carbon dioxide to formate 2) To experimentally measure thermochemical properties, such as hydride donor ability, and use these quantities to optimize catalyst performance in solutions of varying pH 3) To incorporate results from detailed mechanistic and kinetic studies to direct improvements in catalyst design 4) To use thermochemical data from objective 2 to generate predictive models for the properties of new complexes to apply to the development of catalysts for other reductive reactions, with an emphasis on carbon dioxide reduction to methanol Description: Wide-spread implementation of renewable but intermittent energy sources, such as solar, requires the development of efficient methods for energy storage. The high energy density of chemical bonds makes chemical fuels an ideal solution for energy storage. Hydrogen and reduced carbon compounds have been proposed as ideal candidates for chemical fuels. However, the generation of chemical fuels from electricity requires competent electrocatalysts. The proposed research focuses on developing electrocatalysts for the reduction of water to hydrogen, and carbon dioxide to formate. Both products can be used directly as an energy carrier in fuel cells, or as a reductant for more saturated chemical fuels. Hydrogen is the most common fuel used in current commercial fuel cells. Additionally, there is interest in formic acid as a liquid carrier for hydrogen because of its increased storage density and ease of dehydrogenation. Formate is also an intermediate in the sequential reduction of CO 2 to methanol, another potential chemical fuel with high energy storage density. Despite the utility of formate as a chemical fuel or precursor, there are very few examples of electrocatalysts for its production from CO 2 , and even fewer demonstrate high product selectivity. In heterogeneous catalysis, the Sabatier principle is used to generate volcano curves that describe optimal thermochemical properties for key intermediates that result in peak catalytic activity. In most cases, such as hydrogen production and oxidation, the most favorable metals (Pt, Re, Rh, and Ir) are rare and expensive. Molecular inorganic complexes provide an opportunity to use electronic and steric ligand effects to tune the critical thermodynamic parameters of abundant metals to values comparable to key surface intermediates on precious metals. This principle will be applied to the design of aqueous homogeneous catalysts for the reduction of H 2 O and CO 2 optimized to function at specific pH ranges. The critical intermediate in both of these reactions is a metal hydride. The strength of this bond, or hydricity (ΔGH - ) dictates the overall thermodynamics of the reduction of H + to H 2 and the sequential reduction of C1 substrates, such as CO 2 , CO, and H 2 CO (the latter to CH 3 OH). ΔGH - will be systematically measured for a series of first row metal complexes to form predictive models for metal and ligand electronic effects. Benefits and Outcomes: This approach addresses thermodynamic requirements essential for energy-efficient catalyst design and transition state barrier considerations for faster catalysis. The advancements made from this research will include the discovery of efficient, stable, and fast catalysts for hydrogen and formate generation from electricity. The ability to store energy efficiently is critical to the widespread use of renewable energy schemes. This provides a viable solution to produce high energy density fuels for stationary and mobile energy applications. The fundamental research conducted is also directly applicable to the design of catalysts for the generation of further reduced products such as methanol.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Resolving Chemical and Spatial Heterogeneities at Complex Electrochemical Interfaces in Li-Ion Batteries

The high specific capacities of Ni-rich transition metal oxides have garnered immense interest for improving the energy density of Li-ion batteries (LIBs). Despite the potential of these materials, Ni-rich cathodes suffer from interfacial instabilities that lead to crystallographic rearrangement of the active material surface as well as the formation of a cathode electrolyte interphase (CEI) layer on the composite during electrochemical cycling. While changes in crystallographic structure can be detected with diffraction-based methods, probing the chemistry of the disordered, heterogeneous CEI layer is challenging. In this work, we use a combination of ex situ solid-state nuclear magnetic resonance (SSNMR) spectroscopy and X-ray photoemission electron microscopy (XPEEM) to provide chemical and spatial information, on the nanometer length scale, on the CEI deposited on LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) composite cathode films. XPEEM elemental maps offer insight into the lateral arrangement of the electrolyte decomposition products that comprise the CEI and paramagnetic interactions (assessed with electron paramagnetic resonance (EPR) and relaxation measurements) in 13 C SSNMR provide information on the radial arrangement of the CEI from the NMC811 particles outward. Using this approach, here we find that LiF, Li 2 CO 3 , and carboxy-containing structures are directly appended to NMC811 active particles, whereas soluble species detected during in situ 1 H and 19 F solution NMR experiments (e.g., alkyl carbonates, HF, and vinyl compounds) are randomly deposited on the composite surface. We show that the combined approach of ex situ SSNMR and XPEEM, in conjunction with in situ solution NMR, allows spatially-resolved, molecular-level characterization of paramagnetic surfaces and new insights into electrolyte oxidation mechanisms in porous electrode films.

36 MATERIALS SCIENCE↗

Interpreting the Operando XANES of Surface-Supported Subnanometer Clusters: When Fluxionality, Oxidation State, and Size Effect Fight.

X-ray absorption near edge structure (XANES) spectroscopy is widely used for operando catalyst characterization. We show that, for highly fluxional supported nanoclusters, the customary extraction of the oxidation state of the metal from the XANES data by fitting to the bulk standards is highly questionable. The XANES signatures as well as the apparent oxidation state for such clusters arise from a complex combination of many factors, and not only from the chemical composition in reaction conditions (e.g., oxygen content in oxidizing atmosphere). The thermally accessible isomerization and population of several structurally distinct cluster forms, cluster-support interaction, and intrinsic size effects all impact the metal oxidation state and XANES signal. We demonstrate this on copper oxide clusters with different compositions, Cu4Ox(x = 2-5) and Cu5Oy (y = 3, 5), deposited on amorphous alumina and ultrananocrystalline diamond, for which we computed the XANES spectra and compare the results to the experiment. We show in addition that fitting the experimental spectrum to calculated spectra of supported clusters can, in contrast, provide good agreement and insight into the spectrum-composition-structure relation. Experimental XANES interpreted using the proposed fitting scheme shows the partial reduction of Cu oxide clusters at rising temperatures, and pinpoints the specific stoichiometries that dominate in the ensemble of cluster states as the temperature changes.

Zandkarimi, Borna↗

The striking influence of oxophilicity differences in heterometallic Mo–Mn oxide cluster reactions with water

Mixed-metal oxides have proven to be effective catalysts for the hydrogen evolution reaction, often outperforming either of the binary metal oxides. The reactivity of Mn x MoO y - (x = 1, 2; y = 3, 4) clusters toward H 2 O was investigated via time-of-flight mass spectrometry with clear evidence of cluster oxidation and corresponding H 2 production, specifically for Mn x MoO 3 - (x = 1, 2) clusters. Unlike previously studied MoxOy- clusters, which assumed a broad distribution of stoichiometries (typically x ≤ y ≤ 3x), both MnMoOy- and Mn 2 MoO y - preferentially formed y = 3 and 4 compositions in significant quantities under our source conditions. The electronic and molecular structures of the Mn x MoO y (x = 1, 2; y = 3, 4) anion and neutral clusters were probed with anion photoelectron spectroscopy and analyzed with supporting density functional theory calculations. Our studies suggest that both metal centers are involved in initial cluster–water complex formation, while Mo is the center that undergoes oxidation; hence, reactivity terminates when Mo is saturated in its highest oxidation state of +6. Across these four clusters, Mn remains relatively reduced and is stable in a high-spin electronic configuration. The preferential reactivity of water molecules toward the Mo center rather than Mn is rationalized by the much lower relative oxophilicity of Mn.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Perspective—Emergent Phases in Rare Earth Nickelate Heterostructure

The prediction of high T c superconductivity in layers of LaNiO 3 through orbital engineering has led to extensive research efforts over the last fifteen years. During this period, a plethora of thin films and heterostructures based rare-earth nickelate family with perovskite structure has been synthesized and explored. Here, in this short perspective, we briefly review the complexity of bulk RENiO 3 , spotlighting several recent findings of emergent phenomena in heterostructures containing the interface between RENiO 3 and another transition metal oxide. Finally, we outline potentially interesting future directions linked to time-domain dynamics to harness new Mott and topological phases in artificial structures of RENiO 3 .

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Heterogeneous Integration of Flipped Oxide Heterostructure Membranes for Nanoelectronics

Freestanding complex oxide membranes enable the release and transfer of epitaxial films, offering new design freedoms for next‐generation electronics. While the LaAlO 3 /SrTiO 3 (LAO/STO) heterostructure exhibits remarkable tunable conductivity at its interface, the active interface remains buried beneath the substrate, limiting access to this functionality. Here, we demonstrate how the LAO/STO heterostructure, in membrane form, can be flipped and precisely positioned on silicon and other platforms using polymer‐free micromanipulation. The transferred membranes preserve atomically smooth surfaces, high crystallinity, and key electronic properties. Through the 44‐nm insulating STO layer, ultra‐low‐voltage electron‐beam lithography (ULV‐EBL) writes conductive nanostructures at the now‐accessible STO/LAO interface, offering the potential to function as programmable local gates that modulate charge carriers in the underlying silicon. The platform establishes a general strategy for integrating complex oxide heterostructures with semiconductors, quantum materials, and flexible substrates, enabling new architectures for reprogrammable nanoelectronic devices.

36 MATERIALS SCIENCE↗

Low-temperature grapho-epitaxial La-substituted BiFeO 3 on metallic perovskite

Bismuth ferrite has garnered considerable attention as a promising candidate for magnetoelectric spin-orbit coupled logic-in-memory. As model systems, epitaxial BiFeO 3 thin films have typically been deposited at relatively high temperatures (650–800 °C), higher than allowed for direct integration with silicon-CMOS platforms. Here, we circumvent this problem by growing lanthanum-substituted BiFeO 3 at 450 °C (which is reasonably compatible with silicon-CMOS integration) on epitaxial BaPb 0.75 Bi 0.25 O 3 electrodes. Notwithstanding the large lattice mismatch between the La-BiFeO 3 , BaPb 0.75 Bi 0.25 O 3 , and SrTiO 3 (001) substrates, all the layers in the heterostructures are well ordered with a [001] texture. Polarization mapping using atomic resolution STEM imaging and vector mapping established the short-range polarization ordering in the low temperature grown La-BiFeO 3 . Current-voltage, pulsed-switching, fatigue, and retention measurements follow the characteristic behavior of high-temperature grown La-BiFeO 3 , where SrRuO 3 typically serves as the metallic electrode. These results provide a possible route for realizing epitaxial multiferroics on complex-oxide buffer layers at low temperatures and opens the door for potential silicon-CMOS integration.

36 MATERIALS SCIENCE↗

Electronic band contraction induced low temperature methane activation on metal alloys

The catalytic conversion of methane under mild conditions is an appealing approach to selectively produce value-added products from natural gas. Catalysts which can chemisorb methane can potentially overcome challenges associated with its high stability and achieve facile activation. Although transition metals can activate C–H bonds, chemisorption and low-temperature conversion remain elusive on these surfaces. The broad electronic bands of metals can only weakly interact with the methane orbitals, in contrast to specific transition metal oxide and supported metal cluster surfaces which are now recognized to form methane σ-complexes. Here, we report methane chemisorption can, remarkably, occur on metal surfaces via electronic band contraction and localization from metal alloying. From a broad screening including single atom and intermetallic alloys in various substrates, we find early transition metals as promising metal solutes for methane chemisorption and low-temperature activation. These findings demonstrate a combinatorial diversity of possible candidates in earth abundant metal alloys with this attractive catalytic behavior.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Extreme tensile strain states in La 0.7 Ca 0.3 MnO 3 membranes

A defining feature of emergent phenomena in complex oxides is the competition and cooperation between ground states. In manganites, the balance between metallic and insulating phases can be tuned by the lattice; extending the range of lattice control would enhance the ability to access other phases. We stabilized uniform extreme tensile strain in nanoscale La 0.7 Ca 0.3 MnO 3 membranes, exceeding 8% uniaxially and 5% biaxially. Uniaxial and biaxial strain suppresses the ferromagnetic metal at distinctly different strain values, inducing an insulator that can be extinguished by a magnetic field. Electronic structure calculations indicate that the insulator consists of charge-ordered Mn 4+ and Mn 3+ with staggered strain-enhanced Jahn-Teller distortions within the plane. This highly tunable strained membrane approach provides a broad opportunity to design and manipulate correlated electron states.

36 MATERIALS SCIENCE↗

Harvesting Energy from Wastewater by Converting Sewage

This project aims were to develop and demonstrate a scalable, integrated process to convert sewage sludge into renewable natural gas (RNG), enabling wastewater treatment plants (WWTPs) to become net energy producers. The system proposal integrates autothermal hydrothermal liquefaction (AT-HTL), supercritical salt precipitation (SCSP), and hydrothermal gasification (HTG), collectively forming the Supercritical Sludge-to-Gas (SC-S2G) platform. Initially, batch hydrothermal liquefaction reactions were used to screen sewage sludge using AT-HTL (later termed RI-HTL) conversion to biocrude, aqueous and char phases compared to hydrothermal liquefaction (HTL). Significant improvement in biocrude yield using peroxide addition at O:C ratio of 0.05 and under conditions of 300°C for 10 minutes gave 57% biocrude yield and 85% fluid carbon yield (biocrude plus aqueous), while minimizing the loss of carbon to char solids (~7%). Hence, RI-HTL was shown to be effective for conversion of real sewage sludge. The corrosion of the alloy reactor tubes or vessels is an important factor when developing a process that includes an oxidant and a chemically complex feed like sewage sludge. We investigated the corrosion rates on metal alloys at 350°C for 240 hours. Corrosion rates of 0.21 and 0.26 mpy for 304L and 316L stainless steel were measured respectively. The corrosion information obtained in this investigation was utilized by PNNL for design, materials sourcing and construction of the pilot scale continuous flow system.

09 BIOMASS FUELS↗

Illuminating the Photophysics of Oxygen Atom Transfer in Rare Earth Metal-Organic Complexes

Industrial separations of rare earth metals are reliant on selectivity based on ionic radii, which are time, energy, and resource consuming.1 The unique and discontinuous manifold of energy states associated with the f-electron configurations of the rare earth ions2 offer an opportunity to overcome some of these limitations by incorporating light into the separation process. Here, we use transient absorption spectroscopy to understand the differences in mechanism of light-initiated oxygen atom transfer (OAT) in yttrium (Y) and dysprosium (Dy) rare earth complexes. These metal-organic complexes are functionalized with hexfluoroacetyl-acetonate (hfac) and 4-methylmorpholine-N-oxide (NMMO). After light absorption in the presence of triphenyl phosphine (TPP), the NMMO in the Y-NMMO complex is replaced by the TPPO OAT reaction product. Because the Dy f-electron manifold is accessible to the ligand excited states, while there are no accessible states associated with f-electrons for Y, there are significant differences in reactivity. Transient absorption spectroscopy (TAS) was used to monitor changes after 340 nm photoexcitation of Dy/Y-NMMO or the product complex Dy/Y-TPPO. TAS is a pump-probe technique where a white light probe pulse is delayed relative to a visible pump pulse, which photoexcites a sample. Differences between the ground and excited states are monitored over time. With TAS, we access time scales from 100 fs-400 us to determine the photophysics of the complexes of interest. Photoexcitation of Y-NMMO (Fig. 1A) creates a broad photoinduced absorption (PIA) that evolves into a sharp positive feature over 4.2 ps centered at 450 nm. A secondary feature centered at 550 nm grows in with a 200 ps time constant and remains through the 5 ns time window of our experiment. Control experiments for Y-TPPO reveal that the feature at 450 nm is due to internal dynamics of the hfac ligand, while the 550 nm shoulder is due to the presence of the NMMO. Comparing kinetics at 550 nm for Y-NMMO and Dy-NMMO (Fig. 1B) shows that while Y exhibits a distinct growth in the NMMO feature, the Dy decays almost completely within 5 ns. Control experiments with Dy-TPPO prove that the ligand excited states centered on the hfac ligand are deactivated via energy transfer to the Dy manifold within 200 ps. This deactivation leads to significant differences in OAT reactivity between Y and Dy.

CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSICS↗

Tailoring Redox Active Ligands for Probing the Reactivity of Actinides

With this project, we aim to further enhance our understanding of fundamental f-element chemistry, including electronic structure and bonding behaviors. Key project goals include the characterization of actinide complexes bearing redox-active ligands, including those of lower-oxidation state uranium, and examining how structural changes to the ligand and coordination sphere affect structure and bonding. Redox-active and redox non-innocent ligands have been used widely in transition metal chemistry, but uranium complexes with redox-active ligands are surprisingly rare. We recently reported the synthesis of the redox-active ligand, “phen-BIAN” (N,N’-bis(iminophenol)acenaphthene), in an investigation of the electronic behavior of uranium and other actinides. This ligand framework borrows features from two classes of Schiff base ligands—the tetradentate O-N-N-O binding pocket from salens, and the redox-active α-diimine unit and backbone from Ar-BIANs (N,N’-bis[(aryl)imino]acenaphthenes, which can accept up to four electrons upon reduction. To continue this work, the electronics of uranyl and thorium complexes will be probed using the reduced forms of these ligands, using these in the preparation of lower-oxidation state and non-oxo uranium complexes. Additional members of the phen-BIAN family will be synthesized, including naphthol and thiol derivative. With these we can characterize the influence of substitutent groups on the redox activity, coordination geometry, and covalent interactions. The work proposed here entails extensive preparation, structural and spectroscopic characterization, of an array of actinide complexes. This will allow us to address probative questions about the nature of actinide bonding, the degree of covalency, the validity of lanthanides as models for the actinides, hard-soft interactions, magnetic interactions between metals in bimetallic complexes and what combination of electronic and steric affects produce an actinide selective ligand. The latter will assist greatly in providing a benchmark against which to compare and evaluate the distinct behaviors exhibited by 5f-element complexes. This will enable us to learn about the differences in binding between the 4f lanthanides and the 5f elements like uranium and plutonium. Such difference in binding can be exploited in separations and the development of new materials.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗