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At least 811 records · Page 45
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Electronic Rearrangement in Steps of Reductive Elimination of Polar Electrophiles Leads to Refinement of Redox Events

The oxidative addition/reductive elimination of polar molecules such as methyl iodide at late metal centers has a strongly supported $S_{N^2}$ mechanism for many key organometallic complexes, including important industrial catalysts. In the reductive elimination direction, it is proposed that a ligand initially dissociates, typically a halide, followed by subsequent nucleophilic attack at the ligand trans to the now vacant site. The prevailing view is the metal reduction occurs upon transferring the electrophile in the $S_{N^2}$ step. Herein, we report the use of an ensemble of computational techniques to characterize the electronic structure of the reactants and intermediates along this reductive elimination pathway. These calculations demonstrate, unexpectedly, that the initiating loss of an anionic ligand from the octahedral highly oxidized structure leads to an electronic rearrangement that shifts electron density from the apical ligand back toward the metal resulting in an inversion of the electron flow between the metal and apical ligand. The anisotropic shift in electron density to the metal disproportionately affects the apical position, which is best described as a Pt → Me dative bond. With this Pt → Me bonding description, our interpretation of the IUPAC oxidation state formalism would assign the intermediate as Pt ΙΙ . Although counterintuitive, the formal and functional reduction of the metal thus occurs upon halide dissociation.

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

Inverse iron oxide/metal catalysts from galvanic replacement

Key chemical transformations require metal and redox sites in proximity at interfaces; however, in traditional oxide-supported materials, this requirement is met only at the perimeters of metal nanoparticles. We report that galvanic replacement can produce inverse FeO x /metal nanostructures in which the concentration of oxide species adjoining metal domains is maximal. The synthesis involves reductive deposition of rhodium or platinum and oxidation of Fe 2+ from magnetite (Fe 3 O 4 ). We discovered a parallel dissolution and adsorption of Fe 2+ onto the metal, yielding inverse FeO x -coated metal nanoparticles. This nanostructure exhibits the intrinsic activity in selective CO 2 reduction that simple metal nanoparticles have only at interfaces with the support. By enabling a simple way to control the surface functionality of metal particles, our approach is not only scalable but also enables a versatile palette for catalyst design.

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

JSC Metal Finishing Waste Minimization Methods

THe paper discusses the following: Johnson Space Center (JSC) has achieved VPP Star status and is ISO 9001 compliant. The Structural Engineering Division in the Engineering Directorate is responsible for operating the metal finishing facility at JSC. The Engineering Directorate is responsible for $71.4 million of space flight hardware design, fabrication and testing. The JSC Metal Finishing Facility processes flight hardware to support the programs in particular schedule and mission critical flight hardware. The JSC Metal Finishing Facility is operated by Rothe Joint Venture. The Facility provides following processes: anodizing, alodining, passivation, and pickling. JSC Metal Finishing Facility completely rebuilt in 1998. Total cost of $366,000. All new tanks, electrical, plumbing, and ventilation installed. Designed to meet modern safety, environmental, and quality requirements. Designed to minimize contamination and provide the highest quality finishes.

Sullivan, Erica↗
DOE OSTI2023

Engineered Catalyst Support with Improved Durability at Higher Weight Percentage of Platinum

Proton Exchange Membrane (PEM) fuel cells are a suitable electrochemical power source for heavy duty vehicle (HDV) applications due to their high efficiency and durability. The cathode of the fuel cell uses a higher geometric loading of platinum (∼0.2 to 0.4 mg Pt /cm 2 ) for the electrocatalysis of the kinetically sluggish Oxygen Reduction Reaction (ORR) which requires higher weight percent loading of the metal (∼50%) on the carbon support to decrease the catalyst layer thickness and hence, the reactant transport losses. The conventionally used supports for platinum catalyst, such as the KetjenBlack TM type high surface area carbon (HSC) features limited mesopore area for the dispersion of Pt nanoparticles leading to increased aggregation and poor durability. Here, we show a new class of carbon materials known as the Engineered Catalyst Support (ECS) developed by Pajarito Powder with higher mesopore fraction for the dispersion of higher weight percentage of Pt nanoparticles. ECS materials can disperse up to 50% Pt by weight of the catalyst thereby enabling lower catalyst layer thickness with higher performance retained after durability test. A comprehensive set of physico-chemical and electrochemical studies in membrane electrode assembly (MEA) are reported to understand the performance and durability of Pt/ECS catalysts.

08 HYDROGEN↗
NASA NTRS1996

Nonlinear Dynamics of a Foil Bearing Supported Rotor System: Simulation and Analysis

Foil bearings provide noncontacting rotor support through a number of thin metal strips attached around the circumference of a stator and separated from the rotor by a fluid film. The resulting support stiffness is dominated by the characteristics of the foils and is a nonlinear function of the rotor deflection. The present study is concerned with characterizing this nonlinear effect and investigating its influence on rotordynamical behavior. A finite element model is developed for an existing bearing, the force versus deflection relation characterized, and the dynamics of a sample rotor system are studied. Some conclusions are discussed with regard to appropriate ranges of operation for such a system.

Li, Feng↗
DOE OSTI2022

Performance of biochar assisted catalysts during hydroprocessing of non-edible vegetable oil: Effect of transition metal source on catalytic activity

Biochar-supported catalysts were developed from nickel (Ni) - and cobalt (Co)- nitrates and hydroxides and tested for the hydrotreatment of carinata oil. Nitrate-based (from water-soluble salts) and hydroxide-based (from water-insoluble salts) catalysts of Ni and Co were prepared via wetness impregnation and aqueous dispersion methods, respectively. The catalysts were characterized using various tools such as, confocal XRF, BET specific surface area analyzer, NH3-TPD, and SEM-EDS. Synchroton method showed nitrate-sourced metals were dispersed mostly in the pores while, the hydroxide-sourced metals were distributed mainly on the catalyst surface. C = C saturation and cracking of triglycerides, decarboxylation, and hydrogenation of aromatic structures appeared to be dominant on the hydroxides of transition metals, hence took place on catalyst surface. Methanation and dehydrogenation (thus aromatization), however, seemed to be a pore phenomenon, catalyzed more over nitrate-based catalysts. A reaction network was proposed based on chemical analysis of upgraded carinata oil and erucic acid model compound. Catalytic cracking followed by hydrotreatment performed better in terms of fuel properties than other approaches in this study.

Biochar catalysts↗
DOE OSTI2022

A General Route to Flame Aerosol Synthesis and In Situ Functionalization of Mesoporous Silica

Abstract Mesoporous silica is a versatile material for energy, environmental, and medical applications. Here, for the first time, we report a flame aerosol synthesis method for a class of mesoporous silica with hollow structure and specific surface area exceeding 1000 m 2 g −1 . We show its superior performance in water purification, as a drug carrier, and in thermal insulation. Moreover, we propose a general route to produce mesoporous nanoshell‐supported nanocatalysts by in situ decoration with active nanoclusters, including noble metal (Pt/SiO 2 ), transition metal (Ni/SiO 2 ), metal oxide (CrO 3 /SiO 2 ), and alumina support (Co/Al 2 O 3 ). As a prototypical application, we perform dry reforming of methane using Ni/SiO 2 , achieving constant 97 % CH 4 and CO 2 conversions for more than 200 hours, dramatically outperforming an MCM‐41 supported Ni catalyst. This work provides a scalable strategy to produce mesoporous nanoshells and proposes an in situ functionalization mechanism to design and produce flexible catalysts for many reactions.

Liu, Shuo↗
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↗
NASA NTRS2010

The NASA Langley Isolator Dynamics Research Lab

The Isolator Dynamics Research Lab (IDRL) is under construction at the NASA Langley Research Center in Hampton, Virginia. A unique test apparatus is being fabricated to support both wall and in-stream measurements for investigating the internal flow of a dual-mode scramjet isolator model. The test section is 24 inches long with a 1-inch by 2-inch cross sectional area and is supplied with unheated, dry air through a Mach 2.5 converging-diverging nozzle. The test section is being fabricated with two sets (glass and metallic) of interchangeable sidewalls to support flow visualization and laser-based measurement techniques as well as static pressure, wall temperature, and high frequency pressure measurements. During 2010, a CFD code validation experiment will be conducted in the lab in support of NASA s Fundamental Aerodynamics Program. This paper describes the mechanical design of the Isolator Dynamics Research Lab test apparatus and presents a summary of the measurement techniques planned for investigating the internal flow field of a scramjet isolator model.

Middleton, Troy F.↗
DOE OSTI2021

Microwave-assisted conversion of methane over H-(Fe)-ZSM-5: Evidence for formation of hot metal sites

We report microwave-assisted catalysis offers great promise as an “intensified” technology for chemical processing. The present study investigates microwave-assisted direct conversion of methane with focus on the design and evaluation of microwave-sensitive H-(Fe)ZSM-5 catalysts for the existence of hotspot formation. Isomorphous substituted H-(Fe)ZSM-5 catalysts are tuned to identify key design parameters that control their microwave sensitivity. Increasing the amount of Al and Fe substitution in the zeolite lattice is found to result in higher microwave sensitivity due to improved dielectric properties and hence facilitated microwave heating of the catalyst bed. Comparison between the performance of these catalysts in a conventional thermally-heated (CH) fixed-bed and a microwave (MW) reactor allows identification of the effect of microwave irradiation on the catalyst activity. Methane conversion is drastically enhanced at MW conditions (from 3% at CH conditions to 40% at MW conditions), indicating accelerated methane activation over the metal site and hence suggesting a hot metal site despite much lower catalyst bulk temperature measured in the microwave reactor. The existence of metal hotspot formation is further supported by the reaction product distribution and spent catalyst analysis. At MW conditions, C 2 (ethane and ethylene) and coke (mainly carbon nanotubes and nanofibers) selectivity are much higher at the cost of aromatics make compared to CH conditions. This can be explained by reduced aromatization activity at the Brønsted acid sites of the zeolite due to its lower relative temperature of the zeolite. The much-enhanced metal aggregation observed in the spent catalyst from the MW reactor along with the distribution of coke species further confirms the existence of selective heating (i.e. hotspot formation) occurring at the active metal site in the catalyst at MW conditions.

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

A Uranium(II) Arene Complex That Acts as a Uranium(I) Synthon

We report two-electron reduction of the amidate-supported U(III) mono(arene) complex U(TDA) 3 (2) with KC 8 yields the anionic bis(arene) complex [K[2.2.2]cryptand][U(TDA) 2 ] (3) (TDA = N-(2,6-di-isopropylphenyl)pivalamido). EPR spectroscopy, magnetic susceptibility measurements, and calculations using DFT as well as multireference CASSCF methods all provide strong evidence that the electronic structure of 3 is best represented as a 5f 4 U(II) metal center bound to a monoreduced arene ligand. Reactivity studies show 3 reacts as a U(I) synthon by behaving as a two-electron reductant toward I 2 to form the dinuclear U(III)–U(III) triiodide species [K[2.2.2]cryptand][(UI(TDA) 2 ) 2 (μ-I)] (6) and as a three-electron reductant toward cycloheptatriene (CHT) to form the U(IV) complex [K[2.2.2]cryptand][U(η 7 -C 7 H 7 )(TDA) 2 (THF)] (7). The reaction of 3 with cyclooctatetraene (COT) generates a mixture of the U(III) anion [K[2.2.2]cryptand][U(TDA) 4 ] (1-crypt) and U(COT) 2 , while the addition of COT to complex 2 instead yields the dinuclear U(IV)–U(IV) inverse sandwich complex [U(TDA) 3 ] 2 (μ-η 8 :η 3 -C 8 H 8 ) (8). Two-electron reduction of the homoleptic Th(IV) amidate complex Th(TDA) 4 (4) with KC 8 gives the mono(arene) complex [K[2.2.2]cryptand][Th(TDA) 3 (THF)] (5). The C–C bond lengths and torsion angles in the bound arene of 5 suggest a direduced arene bound to a Th(IV) metal center; this conclusion is supported by DFT calculations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2009

Oxygen Production from Lunar Regolith using Ionic Liquids

The objective of this work and future follow-on work is to develop a safe, efficient, and recyclable method for oxygen and/or metals extraction from lunar regolith, in support of establishing a manned lunar outpost. The approach is to solubilize the oxides that comprise lunar regolith in media consisting of ionic liquids (ILs) and/or their mixtures at temperatures at or below 300 C. Once in solution, electrolysis can either be performed in-situ to generate oxygen at the anode and hydrogen and/or metals (silicon, iron, aluminum, titanium, etc.) at the cathode. Alternatively, the water that is generated during the solubilization process can be distilled out and condensed into a separate IL and then electrolysized to produce hydrogen and oxygen. In the case of lunar regolith, this method could theoretically produce 44g oxygen per 100g of regolith. The oxygen can be used for human life support and/or as an oxidizer for rocket fuels, and the metals can be used as raw materials for construction and/or device fabrication. Moreover, the hydrogen produced can be used to re-generate the acidic medium, which can then be used to process additional regolith, thereby making the materials recyclable and limiting upmass requirements. An important advantage of IL acid systems is that they are much "greener" and safer than conventional materials used for regolith processing such as sulfuric or hydrochloric acids. They have very low vapor pressures, which means that they contain virtually no toxic and/or flammable volatile content, they are relatively non-corrosive, and they can exhibit good stability in harsh environments (extreme temperatures, hard vacuum, etc.). Furthermore, regolith processing can be achieved at lower temperatures than other processes such as molten oxide electrolysis or hydrogen reduction, thereby reducing initial power requirements. Six ILs have been synthesized and tested for their capability to dissolve lunar simulant, and for electrochemical and thermal stability. The results showed that ILs can be very efficient electrolytes; in particular IL/phosphoric-acid mixtures appear extremely promising for solubilizing lunar simulant. Results from preliminary experiments for distillation of water produced from the oxygen within the metal oxides of the simulant and the hydrogen from the acid indicates that over 75% of the oxygen from the simulant can be harvested as water at a temperature of 150 C. A method for collection of oxygen from electrolysis of the water derived from solubilizing simulant was developed by using a liquid nitrogen trap to liquefy and collect the oxygen. Although precise quantification of the liquid oxygen trapped is difficult to obtain, the amount of hydrogen and oxygen collected from electrolysis of water in this system was greater than 98%. This set-up also included a portable mass spectrometer for the identification of gases released from electrolysis cells. Regeneration of ILs through re-protonation was also demonstrated. Four sequential re-generations of an IL following solubilization of simulant showed no significant differences in amounts of simulant dissolved. Follow-on work for this project should include more studies of IL/phosphoric acid systems. Also, much more work is necessary for defining methods for electrolysis and purification of metals from regolith solubilized in ILs, and for developing a system to use the produced hydrogen to regenerate the spent IL. Finally, design and development of flight breadboard and prototype hardware is required.

Paley, Mark Steven↗
DOE OSTI2024

Nanoscale visualization and spectral fingerprints of the charge order in ScV 6 Sn 6 distinct from other kagome metals

Charge density waves (CDWs) in kagome metals have been tied to many exotic phenomena. Here, using spectroscopic-imaging scanning tunneling microscopy and angle-resolved photoemission spectroscopy, we study the charge order in kagome metal ScV 6 Sn 6 . The similarity of electronic band structures of ScV 6 Sn 6 and TbV 6 Sn6 (where charge ordering is absent) suggests that charge ordering in ScV 6 Sn 6 is unlikely to be primarily driven by Fermi surface nesting of the Van Hove singularities. In contrast to the CDW state of cousin kagome metals, we find no evidence supporting rotation symmetry breaking. Differential conductance dI/dV spectra show a partial gap Δ 1 CO ≈ 20 meV at the Fermi level. Interestingly, dI/dV maps reveal that charge modulations exhibit an abrupt phase shift as a function of energy at energy much higher than Δ 1 CO , which we attribute to another spectral gap. Our experiments reveal a distinctive nature of the charge order in ScV 6 Sn 6 with fundamental differences compared to other kagome metals.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Impact of Carbon Support Structure on the Durability of PtCo Electrocatalysts

High performing, low-Pt content fuel cell membrane electrode assemblies (MEAs) are critical to the economic viability of proton exchange membrane fuel cells (PEMFCs) for the transportation industry. Considerable research has been conducted to reduce the Pt content in fuel cells, leading to the development of transition metal alloys, such as Platinum-Cobalt (PtCo). The degree of degradation of PtCo catalysts can be impacted by the catalyst metal itself and its interactions with the carbon support. Several low-loaded PtCo MEAs were fabricated, with various combinations of porous and solid carbon cathode catalyst supports. The MEAs were subjected to an accelerated stress test (AST), and the catalyst degradation characterized using electrochemical, X-ray scattering, and electron microscopy techniques. Porous supports retain more of their electrochemically-active surface area (ECSA) and demonstrate higher performance after the AST. Overall, this is believed to be due to the ability of the porous supports to trap the metal particles within the pores, slowing their dissolution/precipitation, and agglomeration.

25 ENERGY STORAGE↗
DOE OSTI2020

FY20 Progress Report on FIPD Development and User Support

The DOE Advanced Reactor Technologies program has supported efforts to recover and preserve metallic fuel data generated throughout the past fast reactor R&D programs. Those efforts have focused on establishing databases for information from the experiments conducted during the Integral Fast Reactor program including data generated at EBR-II, FFTF, and TREAT reactors, as well as out of pile transient testing data. These databases are essential for future-licensing activities of metallic fuel based advanced fast reactors. This report describes the EBR-II Fuels Irradiation & Physics Database (FIPD) development, content updates, and user support during the current fiscal year (FY20). Future plans are also provided.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS2013

Chandra Grating Spectroscopy of Three Hot White Dwarfs

High-resolution soft X-ray spectroscopic observations of single hot white dwarfs are scarce. With the Chandra Low-Energy Transmission Grating, we have observed two white dwarfs, one is of spectral type DA (LB1919) and the other is a non-DA of spectral type PG1159 (PG1520+525). The spectra of both stars are analyzed, together with an archival Chandra spectrum of another DA white dwarf (GD246). Aims. The soft X-ray spectra of the two DA white dwarfs are investigated in order to study the effect of gravitational settling and radiative levitation of metals in their photospheres. LB1919 is of interest because it has a significantly lower metallicity than DAs with otherwise similar atmospheric parameters. GD246 is the only white dwarf known that shows identifiable individual iron lines in the soft X-ray range. For the PG1159 star, a precise effective temperature determination is performed in order to confine the position of the blue edge of the GW Vir instability region in the HRD. Methods. The Chandra spectra are analyzed with chemically homogeneous as well as stratified NLTE model atmospheres that assume equilibrium between gravitational settling and radiative acceleration of chemical elements. Archival EUV and UV spectra obtained with EUVE, FUSE, and HST are utilized to support the analysis. Results. No metals could be identified in LB1919. All observations are compatible with a pure hydrogen atmosphere. This is in stark contrast to the vast majority of hot DA white dwarfs that exhibit light and heavy metals and to the stratified models that predict significant metal abundances in the atmosphere. For GD246 we find that neither stratified nor homogeneous models can fit the Chandra spectrum. The Chandra spectrum of PG1520+525 constrains the effective temperature to T(sub eff) = 150 000 +/- 10 000 K. Therefore, this nonpulsating star together with the pulsating prototype of the GWVir class (PG1159-035) defines the location of the blue edge of the GWVir instability region. The result is in accordance with predictions from nonadiabatic stellar pulsation models. Such models are therefore reliable tools to investigate the interior structure of GW Vir variables. Conclusions. Our soft X-ray study reveals that the understanding of metal abundances in hot DA white dwarf atmospheres is still incomplete. On the other hand, model atmospheres of hydrogen-deficient PG1159-type stars are reliable and reproduce well the observed spectra from soft X-ray to optical wavelengths.

Adamczak, J.↗