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At least 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Electrochemical Nickel-Catalyzed Asymmetric Hydrogenation of C═C Bonds Facilitated by a Proton-Coupled Electron Transfer Mediator

Enantioselective hydrogenation of C═C bonds is foundational to asymmetric synthesis, yet its adaptation to electrochemical methods has been limited by challenges in achieving chemoselectivity versus the hydrogen evolution reaction (HER). In this article, we present a modular electrochemical strategy that merges chiral nickel catalysis with a cobaltocene-derived proton-coupled electron transfer (PCET) mediator to enable the asymmetric hydrogenation of α,β-unsaturated carbonyl compounds. Under optimized conditions, a range of substrates featuring diverse amide functionalities and substitution patterns are hydrogenated in high yields (up to 95%) and enantioselectivities (up to 98% ee). The results described highlight the potential benefits of mediator-assisted, fixed-potential electrocatalysis in selective, stereocontrolled hydrogenation under mild conditions.

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

Hydrocyclization/Defluorination of CF 3 ‐Substituted Acrylamides: Insights from Kinetics of Hydrogen Atom Transfer

Abstract The introduction of F‐containing groups into organic molecules can significantly alter their physical and chemical properties. Particularly, gem ‐difluoroalkenes serve as versatile precursors for a broad variety of organofluorine compounds, commonly used in agrochemicals, pharmaceuticals, and materials science. Based on the kinetics of H• transfer to acrylamide ( k H = 2.28 × 10 −4 M −1 s −1 at 300 K in toluene), the study describes a nickel‐hydride‐(or Li[BEt 3 H]) initiated hydrocyclization/defluorination of CF 3 ‐substituted acrylamides, offering alternative access to 4‐fluorovinyl‐substituted 2‐pyrrolidones (Seletracetam derivatives that are antiepileptic drug candidates). This process proceeds with high yields and remarkable chemo‐ and regioselectivity. The hydrocyclization/defluorination can be initiated by either H• or H – transfer, followed by a 5‐exo‐trig cyclization and subsequent fluorine elimination. The strategy has been applied in the late‐stage functionalization of drug molecules, providing a valuable tool in the synthesis of pharmaceutical compounds.

Wan, Yanjun [College of Pharmaceutical Sciences Zh↗
NASA NTRS2009

Effects of Hypervelocity Impacts on Silicone Elastomer Seals and Mating Aluminum Surfaces

While in space silicone based elastomer seals planned for use on NASA's Crew Exploration Vehicle (CEV) are exposed to threats from micrometeoroids and orbital debris (MMOD). An understanding of these threats is required to assess risks to the crew, the CEV orbiter, and missions. An Earth based campaign of hypervelocity impacts on small scale seal rings has been done to help estimate MMOD threats to the primary docking seal being developed for the Low Impact Docking System (LIDS). LIDS is being developed to enable the CEV to dock to the ISS (International Space Station) or to Altair (NASA's next lunar lander). The silicone seal on LIDS seals against aluminum alloy flanges on ISS or Altair. Since the integrity of a seal depends on both sealing surfaces, aluminum targets were also impacted. The variables considered in this study included projectile mass, density, speed, incidence angle, seal materials, and target surface treatments and coatings. Most of the impacts used a velocity near 8 km/s and spherical aluminum projectiles (density = 2.7 g/cubic centimeter), however, a few tests were done near 5.6 km/s. Tests were also performed using projectile densities of 7.7, 2.79, 2.5 or 1.14 g/cubic centimeter. Projectile incidence angles examined included 0 degrees, 45 degrees , and 60 degrees from normal to the plane of the target. Elastomer compounds impacted include Parker's S0383-70 and Esterline's ELA-SA-401 in the as received condition, or after an atomic oxygen treatment. Bare, anodized and nickel coated aluminum targets were tested simulating the candidate mating seal surface materials. After impact, seals and aluminum plates were leak tested: damaged seals were tested against an undamaged aluminum plate; and undamaged seals were placed at various locations over craters in aluminum plates. It has been shown that silicone elastomer seals can withstand an impressive level of damage before leaking beyond allowable limits. In general on the tests performed to date, the diameter of the crater in either the elastomer, or the aluminum, must be at least as big as 80% to 90% of width of the bulb of the seal before significant leakage occurs.

deGroh, Henry C., III↗
NASA NTRS2009

Effects of Hypervelocity Impacts on Silicone Elastomer Seals and Mating Aluminum Surfaces

While in space silicone based elastomer seals planned for use on NASA's Crew Exploration Vehicle (CEV) are exposed to threats from micrometeoroids and orbital debris (MMOD). An understanding of these threats is required to assess risks to the crew, the CEV orbiter, and missions. An Earth based campaign of hypervelocity impacts on small scale seal rings has been done to help estimate MMOD threats to the primary docking seal being developed for the Low Impact Docking System (LIDS). LIDS is being developed to enable the CEV to dock to the ISS (International Space Station) or to Altair (NASA's next lunar lander). The silicone seal on LIDS seals against aluminum alloy flanges on ISS or Altair. Since the integrity of a seal depends on both sealing surfaces, aluminum targets were also impacted. The variables considered in this study included projectile mass, density, speed, incidence angle, seal materials, and target surface treatments and coatings. Most of the impacts used a velocity near 8 km/s and spherical aluminum projectiles (density = 2.7 g/cubic cm), however, a few tests were done near 5.6 km/s. Tests were also performed using projectile densities of 7.7, 2.79, 2.5 or 1.14 g/cubic cm. Projectile incidence angles examined included 0 deg, 45 deg, and 60 deg from normal to the plane of the target. Elastomer compounds impacted include Parker's S0383-70 and Esterline's ELA-SA-401 in the as received condition, or after an atomic oxygen treatment. Bare, anodized and nickel coated aluminum targets were tested simulating the candidate mating seal surface materials. After impact, seals and aluminum plates were leak tested: damaged seals were tested against an undamaged aluminum plate; and undamaged seals were placed at various locations over craters in aluminum plates. It has been shown that silicone elastomer seals can withstand an impressive level of damage before leaking beyond allowable limits. In general on the tests performed to date, the diameter of the crater in either the elastomer, or the aluminum, must be at least as big as 80% to 90% of width of the bulb of the seal before significant leakage occurs.

deGroh, Henry C., III↗
NASA NTRS1994

Charge efficiency of Ni/H2 cells during transfer orbit of Telstar 4 satellites

The TELSTAR 4 communication satellites being manufactured by Martin Marietta Astro Space (Astro Space) for AT&T are three axis stabilized spacecraft scheduled to be launched on expendable vehicles such as the Atlas or Ariane rockets. Typically, these spacecraft consist of a box that holds the electronics and supports the antenna reflectors and the solar array wings. The wings and reflectors are folded against the sides of the box during launch and the spacecraft is spun for attitude control in that phase; they are then deployed after achieving the final orbit. The launch phase and transfer orbits required to achieve the final geosynchronous orbit typically take 4 to 5 days during which time the power required for command, telemetry, attitude control, heaters, etc., is provided by two 50 AH nickel hydrogen batteries augmented by the exposed outboard solar panels. In the past, this situation has presented no problem since there was a considerable excess of power available from the array. In the case of large high powered spacecraft such as TELSTAR 4, however, the design power levels in transfer orbit approach the time-averaged power available from the exposed surface area of the solar arrays, resulting in a very tight power margin. To compound the difficulty, the array output of the spinning spacecraft in transfer orbit is shaped like a full wave rectified sine function and provides very low charging rates to the batteries during portions of the rotation. In view of the typically low charging efficiency of alkaline nickel batteries at low rates, it was decided to measure the efficiency during a simulation of the TELSTAR 4 conditions at the expected power levels and temperatures on three nickel hydrogen cells of similar design. The unique feature of nickel hydrogen cells that makes the continuous measurement of efficiency possible is that hydrogen is one of the active materials and thus, cell pressure is a direct measure of the state of charge or available capacity. The pressure is measured with a calibrated strain gage mounted on the outside of the pressurized cell.

Fang, W. C.↗
NASA NTRS1979

Primordial retention of carbon by the terrestrial planets

The thermodynamics of graphite, carbide, and carbonate formation in the presence of a solar-composition gas is examined, including the feasibility of producing solid solutions of carbon and carbides in metallic iron-nickel alloy. Gas-phase composition and graphite activities for a very wide range of nebular pressures and temperatures are calculated by a computer program that considers several hundred compounds, particularly all the important gaseous species containing H, C, O, N, S, Cl, P, and F. The results obtained indicate that CH4 and CO would be the dominant carbon compounds under all likely circumstances of temperature and pressure in the solar nebula, that graphite may have been the most abundant carbon species in certain cases, and that direct precipitation of graphite, carbides, or carbonates would have been impossible in the solar nebula. Carbon retention by the terrestrial planets is also investigated.

Lewis, J. S.↗
DOE OSTI2025

Softening of dd excitation in the resonant inelastic x-ray scattering spectra as a signature of Hund's coupling in nickelates

We investigate the effects of Hund's coupling on the resonant x-ray absorption spectra of the recently discovered family of layered nickelate superconductors. We contrast two scenarios depending on the relative strength of the ratio of the effective Hund's coupling ( J H ) to the crystal fields ( Δ ) in these systems. We carry out the cluster and DFT + DMFT simulations of the RIXS signal at the Ni L edge for different values of Hund's coupling. We find the latter dominates for the parent compound while the former becomes important for sufficiently large doping. Our results are consistent with the observations of a softening of a RIXS peak as a function of doping by Rossi [], only when the Hund coupling is sizable. To interpret the results, we separate the theoretical RIXS signal into spin conserving and nonspin conserving channels and conclude that the infinite layer nickelates are in a regime where Δ and J compete effectively and suggest further experimental tests of the theory. Published by the American Physical Society 2025

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS1989

Structural comparison of nickel electrodes and precursor phases

Researchers summarize previous Raman spectroscopic results and discuss important structural differences in the various phases of active mass and active mass precursors. Raman spectra provide unique signatures for these phases, and allow one to distinguish each phase, even when the compound is amorphous to x rays (i.e., does not scatter x rays because of a lack of order and/or small particle size). The structural changes incurred during formation, charge and discharge, cobalt addition, and aging are discussed. The oxidation states and dopant contents are explained in terms of the nonstoichiometric structures.

Cornilsen, Bahne C.↗
DOE OSTI2026

Bioadaptive Ni single atoms unlock high rate microbial electrosynthesis of isopropanol from CO 2

Hybrid systems that integrate electrochemical CO 2 reduction with microbial upgrading offer a viable route to high value organic compounds from CO 2 at ambient conditions. However, electrocatalyst deactivation in microbial growth media remains a key barrier, limiting efficiency and increasing cost. Here we show that a bioadaptive single-atom nickel catalyst (Ni SAC), coupled with genetically engineered Clostridium ljungdahlii, enables robust electrosynthesis of isopropanol (IPA) from CO 2 via a CO-mediated pathway. Instead of relying on H 2 as an electron carrier, the system applies high-rate CO formation in complex growth media, maintaining a tunable CO Faradaic efficiency up to 92%, which is 9.4 to 52.7 times greater than conventional Ag catalysts. This performance supports stable IPA production at current density of 10.8 A/m 2 and production rate of 161.3 mg/L/day. In situ Raman and X-ray absorption spectroscopy, together with theoretical calculations, indicate that the Ni SAC can resist competing organic adsorption and retain its coordination structure during CO 2 reduction in bioelectrolytes, providing a mechanistic basis for the catalyst stability and integrated process performance.

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

Identification and characterization of a small-molecule metallophore involved in lanthanide metabolism

Many bacteria secrete metallophores, low-molecular-weight organic compounds that bind ions with high selectivity and affinity, in order to access essential metals from the environment. Previous work has elucidated the structures and biosynthetic machinery of metallophores specific for iron, zinc, nickel, molybdenum, and copper. No physiologically relevant lanthanide-binding metallophore has been discovered despite the knowledge that lanthanide metals (Ln) have been revealed to be essential cofactors for certain alcohol dehydrogenases across a diverse range of phyla. Here, we report the biosynthetic machinery, the structure, and the physiological relevance of a lanthanophore, methylolanthanin. The structure of methylolanthanin exhibits a unique 4-hydroxybenzoate moiety which has not previously been described in other metallophores. We find that production of methylolanthanin is required for normal levels of Ln accumulation in the methylotrophic bacterium Methylobacterium extorquens AM1, while overexpression of the molecule greatly increases bioaccumulation and adsorption. Our results provide a clearer understanding of how Ln-utilizing bacteria sense, scavenge, and store Ln; essential processes in the environment where Ln are poorly bioavailable. More broadly, the identification of this lanthanophore opens doors for study of how biosynthetic gene clusters are repurposed for additional functions and the complex relationship between metal homeostasis and fitness.

Science & Technology - Other Topics↗
NASA NTRS1990

Structural comparison of nickel electrodes and precursor phases

In this paper the previous Raman spectroscopic results are summarized and important structural differences in the various phases of active mass and active mass precursors are discussed. Raman spectra provide unique signatures for these phases, and allow one to distinguish each phase, even when the compound is amorphous to X-rays (i.e., does not scatter X-rays because of a lack of order and/or small particle size). The structural changes incurred during formation, charge and discharge, cobalt addition, and aging wil be discussed. The oxidation states and dopant contents are explained in terms of the nonstoichiometric structures.

Cornilsen, Bahne C.↗
NASA NTRS1973

Enriched aluminide coatings for dispersion strengthened nickel materials

Improved aluminide/barrier coating combinations for dispersion strengthened nickel materials were investigated. The barrier materials involved alloys with refractory metal content to limit interdiffusion between the coating and the substrate, thereby minimizing void formation. Improved aluminide coatings involved the dispersion of aluminum-rich compounds. Coatings were tested in argon at 1533 K (2300 F) for 100 hours and in cyclic oxidation at 1422 K (2100 F). Two coatings on TDNiCr completed 300 hours of oxidation testing, none on TDNi. Selected coating combinations were evaluated in Mach 1 burner rig testing using JP-4 fuel and air at 1422 K (2100 F) and 1477 K (2200 F) for 350 and 100 hours, respectively. Static oxidation in 1-hour cycles was conducted at 1533 K (2300 F) for 100 hours. For comparison purposes a physical vapor deposition (PVD) NiCrAlY coating was tested concurrently. Only the NiCrA1Y coating survived the 1477 K (2200 F)/100-hour burner rig test and 275 hours of the 350-hour 1422 K (2100 F) test. Elevated temperature exposure reduced room temperature tensile properties but had little effect on elevated temperature properties.

Levinstein, M. A.↗
NASA NTRS1972

Eutectic superalloys strengthened by delta Ni3Cb lamellae, and gamma prime, Ni3Al precipitates.

Bivariant eutectic alloys, located on a liquidus surface within the Ni-Cb-Cr-Al quaternary, were identified which permitted the production of aligned delta Ni3Cb lamellae within a nichrome matrix containing the fcc precipitate gamma prime Ni3Al. The volume fraction of delta and gamma prime could be varied significantly by compositional changes. After directional solidification certain alloys possessed improved ductility and corrosion resistance with respect to the Ni3Al-Ni3Cb eutectic, while their values of tensile and creep strength approached or exceeded those for the Ni3Al-Ni3Cb pseudobinary system. The mechanical properties of the directionally solidified alloy, Ni-19.7 wt % Cb-6.0 wt % Cr-2.5 wt % Al, were evaluated. Its longitudinal strength in tension and creep was found to be superior to all advanced nickel base superalloys. It is thus demonstrated that useful properties for gas turbine airfoil applications can be achieved by reinforcing a strong and tough gamma nichrome matrix containing precipitated gamma prime by a strong lamellar intermetallic compound having greater strength at elevated temperature.

Lemkey, F. D.↗
NASA NTRS1980

Deposition and material response from Mach 0.3 burner rig combustion of SRC 2 fuels

Collectors at 1173K (900 C) were exposed to the combustion products of a Mach 0.3 burner rig fueled with various industrial turbine liquid fuels from solvent refined coals. Four fuels were employed: a naphtha, a light oil, a wash solvent and a mid-heavy distillate blend. The response of four superalloys (IN-100, U 700, IN 792 and M-509) to exposure to the combustion gases from the SRC-2 naphtha and resultant deposits was also determined. The SRC-2 fuel analysis and insights obtained during the combustion experience are discussed. Particular problems encountered were fuel instability and reactions of the fuel with hardware components. The major metallic elements which contributed to the deposits were copper, iron, chromium, calcium, aluminum, nickel, silicon, titanium, zinc, and sodium. The deposits were found to be mainly metal oxides. An equilibrium thermodynamic analysis was employed to predict the chemical composition of the deposits. The agreement between the predicted and observed compounds was excellent. No hot corrosion was observed. This was expected because the deposits contained very little sodium or potassium and consisted mainly of the unreactive oxides. However, the amounts of deposits formed indicated that fouling is a potential problem with the use of these fuels.

Santoro, G. J.↗
NASA NTRS1985

Interdiffusional effects between tungsten fibers and an iron-nickel-base alloy

Tungsten fibers in the INCOLOY 903 alloy were annealed for over 100 hours at 1038 C and 1200 C. It was found that interdiffusion results in the formation of a reaction zone. SEM-EDS probe analysis showed that the chemistries across this zone were constant, suggesting the zone was a compound phase. The composition of the compound was estimated to be that of a mu-type phase. The local chemistry (in atomic percent) at the reaction zone/alloy matrix interface was found to be approximately 8 pct W, 1.2 pct Nb, 40 pct Fe, 14 pct Co, and 36 pct Ni. In addition, recrystallization was observed in both the remaining tungsten fiber and the nearby INCOLOY 903 matrix after annealing at 1200 C, but not at 1038 C. The results of this study suggest that reaction zone growth kinetics can be minimized by the reduction of Co and Fe and the increase of W in the matrix alloy.

Caulfield, T.↗
NASA NTRS1995

Sinterless Fabrication Of Contact Pads On InP Devices

Research has shown that with proper choice of material, low-resistance contact pads deposited on solar cells and other devices by improved technique that does not involve sintering. Research directed at understanding mechanisms involved in contact-sintering process has resulted in identification of special group of materials that includes phosphides of gold, silver, and nickel; specifically, Au(2)P(3), AgP(2), and Ni(3)P. Incorporation of phosphide interlayer substantially reduces resistivity between gold current-carrying layer and indium phosphide substrate. Further research indicated only very thin interlayer of any of these compounds needed to obtain low contact resistance, without subjecting contact to destructive sintering process.

Weizer, Victor G.↗
NASA NTRS1974

An exploratory study of a zirconium-modified, precipitation-strengthened nickel-30 copper alloy

A precipitation-strengthened alloy has been produced through minor additions of zirconium to a base Ni-30Cu alloy. The results of this exploratory study indicate that thermomechanical processing of a solution-treated Ni-30Cu-0.2Zr alloy produced a dispersion of precipitates. The precipitates have been tentatively identified as a Ni5Zr compound. Comparison of the mechanical properties, as determined by testing in air, of the Zr-modified alloy to those of a Ni-30Cu alloy reveals that the precipitation-strengthened alloy has improved tensile properties to 1200 K and improved stress-rupture properties to 1100 K. The oxidation characteristics of the modified alloy appeared to be equivalent to those of the base Ni-30Cu alloy.

Whittenberger, J. D.↗
NASA NTRS1974

High temperature mechanical properties of a zirconium-modified, precipitation- strengthened nickel, 30 percent copper alloy

A precipitation-strengthened Monel-type alloy has been developed through minor alloying additions of zirconium to a base Ni-30Cu alloy. The results of this exploratory study indicate that thermomechanical processing of a solution-treated Ni-30Cu-0.2Zr alloy produced a dispersion of precipitates. The precipitates have been tentatively identified as a Ni5Zr compound. A comparison of the mechanical properties, as determined by testing in air, of the zirconium-modified alloy to those of a Ni-30Cu alloy reveals that the precipitation-strengthened alloy has improved tensile properties to 1200 K and improved stress-rupture properties to 1100 K. The oxidation characteristics of the modified alloy appeared to be equivalent to those of the base Ni-30Cu alloy.

Whittenberger, J. D.↗